WO2019189411A1 - 金属塩化物生成装置、および金属粉体の製造方法 - Google Patents

金属塩化物生成装置、および金属粉体の製造方法 Download PDF

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Publication number
WO2019189411A1
WO2019189411A1 PCT/JP2019/013277 JP2019013277W WO2019189411A1 WO 2019189411 A1 WO2019189411 A1 WO 2019189411A1 JP 2019013277 W JP2019013277 W JP 2019013277W WO 2019189411 A1 WO2019189411 A1 WO 2019189411A1
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Prior art keywords
heating furnace
metal
gas
furnace
chloride
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PCT/JP2019/013277
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English (en)
French (fr)
Japanese (ja)
Inventor
広介 六角
貢 吉田
浅井　剛
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東邦チタニウム株式会社
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Application filed by 東邦チタニウム株式会社 filed Critical 東邦チタニウム株式会社
Priority to KR1020207029466A priority Critical patent/KR102445498B1/ko
Priority to CN201980024083.9A priority patent/CN111936424B/zh
Priority to JP2019529662A priority patent/JP6591129B1/ja
Publication of WO2019189411A1 publication Critical patent/WO2019189411A1/ja

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/16—Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/28—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from gaseous metal compounds
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G3/00—Compounds of copper
    • C01G3/04—Halides
    • C01G3/05—Chlorides
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B1/00—Shaft or like vertical or substantially vertical furnaces
    • F27B1/02—Shaft or like vertical or substantially vertical furnaces with two or more shafts or chambers, e.g. multi-storey
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B7/00—Rotary-drum furnaces, i.e. horizontal or slightly inclined
    • F27B7/02—Rotary-drum furnaces, i.e. horizontal or slightly inclined of multiple-chamber or multiple-drum type
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
    • F27D7/00—Forming, maintaining, or circulating atmospheres in heating chambers
    • F27D7/02—Supplying steam, vapour, gases, or liquids

Definitions

  • One of the embodiments of the present invention relates to a metal chloride generator, a system for producing metal powder, and a method for producing metal powder using the system.
  • Fine metal particles are used in various fields.
  • powders of metals having high conductivity such as copper, nickel, silver, etc. are used as electrons such as internal electrodes of multilayer ceramic capacitors (MLCC).
  • MLCC multilayer ceramic capacitors
  • Several methods for producing such metal powders are known, and an example thereof is a gas phase method. In this method, as disclosed in, for example, Patent Documents 1 and 2, a metal powder is formed by reducing a metal chloride gas in contact with a reducing gas such as hydrogen.
  • One of the embodiments of the present invention is a method capable of stably producing metal powder while preventing damage and destruction of the production apparatus, a metal chloride production apparatus capable of realizing this method, and metal chloride production.
  • An object is to provide a metal powder manufacturing system including an apparatus.
  • One of the embodiments according to the present invention is a metal chloride generator.
  • This metal chloride generating apparatus includes a first heating furnace having a metal inlet for introducing metal, a second heating furnace connected to the first heating furnace, and a first heating furnace. A first heater for heating the furnace and a second heater for heating the second heating furnace are provided.
  • the second heating furnace has a discharge port for discharging a metal chloride gas.
  • the chlorination furnace has a first gas introduction port for introducing a gas containing chlorine, and the first gas introduction port is surrounded by either the first heater or the second heater.
  • One of the embodiments according to the present invention is a metal chloride generator.
  • This metal chloride generator is connected to a first heating furnace and a first heating furnace each having a metal inlet for introducing metal and a gas inlet for introducing nitrogen, and a metal chloride.
  • a second heating furnace having a discharge port for discharging the first heating furnace, a first heater for heating the first heating furnace, a second heater for heating the second heating furnace, and a third heater for heating nitrogen It has a heater.
  • One of the embodiments according to the present invention is a method for producing a metal powder.
  • a metal is reacted with chlorine gas in a chlorination furnace configured to be heated by a first heater and a second heater to produce a metal chloride, and a first provided in the chlorination furnace.
  • the method includes transporting chloride vapor to a reduction furnace by introducing a gas containing chlorine from the gas inlet.
  • the first gas introduction port is surrounded by either the first heater or the second heater.
  • One of the embodiments according to the present invention is a method for producing a metal powder.
  • heated nitrogen is introduced into a chlorinating furnace to react a metal with chlorine gas in the chlorinating furnace to form a metal chloride, and the chlorine vapor is used to reduce the chloride vapor. Including transport to.
  • generation apparatus has a chlorination furnace provided with the 1st heating furnace which has a metal inlet for introducing a metal, and the 2nd heating furnace connected with a 1st heating furnace.
  • the second heating furnace has a discharge port for discharging a metal chloride gas and a first gas introduction port for introducing a gas containing chlorine.
  • One of the embodiments according to the present invention is a metal chloride generator.
  • generation apparatus has a chlorination furnace provided with a 1st heating furnace and a 2nd heating furnace connected with a 1st heating furnace.
  • the first heating furnace has a metal inlet for introducing metal and a first gas inlet for introducing a gas containing chlorine.
  • the second heating furnace has a discharge port for discharging a metal chloride gas.
  • the first gas introduction port is located closer to the connecting portion between the first heating furnace and the second heating furnace than the metal introduction port for introducing metal.
  • the metal chloride generator may further include a first heater that heats the first heating furnace. Further, the first gas introduction port may be surrounded by the first heater.
  • FIG. 1 is a schematic configuration diagram of a metal powder manufacturing system according to one embodiment of the present invention.
  • the typical sectional view of the metal chloride generating device concerning one of the embodiments of the present invention.
  • the typical sectional view of the metal chloride generating device concerning one of the embodiments of the present invention.
  • the typical sectional view of the metal chloride generating device concerning one of the embodiments of the present invention.
  • the typical sectional view of the metal chloride generating device concerning one of the embodiments of the present invention.
  • the typical sectional view of the metal chloride generating device concerning one of the embodiments of the present invention.
  • generation apparatus which concerns on one of embodiment of this invention.
  • the expression “above” or “below” is not particularly specified. As long as there is no other case, another structure is placed directly above or below the structure, and another structure is placed above or below the structure via another structure. Including both cases.
  • the arrangement of the structure is mainly described based on the movement order of the metal chloride gas, and includes the case where the structure called the upper and the structure called the lower are located horizontally, for example. It is.
  • a metal chloride generating apparatus 110 according to one embodiment of the present invention and a metal powder manufacturing system (hereinafter simply referred to as a system) 100 including the same will be described.
  • FIG. 1 shows an outline of the configuration of the system 100.
  • the system 100 includes a metal chloride generator 110 and a reduction furnace 200 as main components.
  • the system 100 may further include a recovery device such as a separation device 300 connected to the reduction furnace 200 and a bag filter connected to the reduction furnace 200 or the separation device 300.
  • the metal chloride generator 110 and the reduction furnace 200 are connected by a first transport pipe 112, and the reduction furnace 200 and the separation apparatus 300 are connected by a second transport pipe 202.
  • the metal chloride generator 110 has one function of generating metal chloride (hereinafter simply referred to as chloride) by the reaction of zero-valent metal and chlorine gas.
  • Chloride exists as a gas (vapor) in the metal chloride generator 110, and part of it exists as a liquid depending on the type of metal and reaction conditions. Chloride vapor is introduced into the reduction furnace 200 through the first transport tube 112.
  • the metal copper, silver, nickel, or the like can be used.
  • the reduction furnace 200 is connected to the first transport pipe 112 and is a gas inlet (fifth gas inlet) for introducing the chloride vapor transported from the metal chloride generator 110 into the reduction furnace 200. 204.
  • the reduction furnace 200 further includes a gas introduction port (sixth gas introduction port) 206 for introducing hydrogen, hydrazine, ammonia, methane, or the like, which is a reducing gas for reducing chloride. Chloride is reduced in the reduction furnace 200, thereby generating metal powder.
  • An inert gas such as nitrogen gas is introduced into the reduction furnace 200 from the outside through a gas introduction port (not shown), and the metal powder generated thereby is cooled and separated through the second transport pipe 202 and the recovery device 300. Transported to the device.
  • the separation device 300 has a function of refining the metal powder by removing aggregates contained in the metal powder and metal sintered products by-produced in the reduction furnace 200. .
  • a recovery device is provided to isolate the purified metal powder from nitrogen gas.
  • the metal chloride generator 110 is provided with a gas inlet for introducing various gases, as will be described later.
  • the metal chloride generator 110 is mainly provided with a chlorination furnace 120 and a chlorination furnace 120 so as to surround the chlorination furnace 120, and includes a first heater 160 and a second heater 162 for heating the chlorination furnace 120.
  • the first heater 160 and the second heater 162 can be controlled independently.
  • the chlorination furnace 120 includes a first heating furnace 122 and a second heating furnace 124.
  • the second heating furnace 124 is located below the first heating furnace 122, but the first heating furnace 122 and the second heating furnace 124 may be arranged horizontally.
  • the reduction furnace 200 may be provided below the first heating furnace 122 and the second heating furnace 124 (see FIG. 1), or these may be disposed horizontally.
  • the inner diameter of the connecting portion 123 between the first heating furnace 122 and the second heating furnace 124 is smaller than the other parts, but as shown in FIG. 3, the first heating furnace 122 is used.
  • the inner diameter of the chlorination furnace 120 may be the same from the first to the second heating furnace 124. Alternatively, the inner diameters of the first heating furnace 122 and the second heating furnace 124 may be different.
  • the chlorination furnace 120 may include a partition member 126 that separates the first heating furnace 122 and the second heating furnace 124 (see FIG. 3). That is, the chlorination furnace 120 may include a first heating furnace 122 and a second heating furnace 124 connected to the first heating furnace 122 by the partition member 126.
  • the partition member 126 is provided with at least one opening, so that the gas introduced into the first heating furnace 122 and the second heating furnace 124 and the vapor of chloride generated in the partition member 126 Can pass through.
  • the number, size, and arrangement of the holes may be appropriately designed in consideration of the reaction conditions, the vapor pressure of chloride, the shape and size of the metal used, and the like.
  • FIG. 3 shows a mode in which the metal is arranged as pellets 114 on the partition member 126 in the first heating furnace 122.
  • Quartz, ceramic, etc. can be used as the material used for the chlorination furnace 120, and can be selected in consideration of the melting point of the metal used and its chloride.
  • Examples of the material used for the partition member 126 include metal or metalloid oxides such as quartz, alumina, and zirconia, ceramics, nitrides such as boron nitride, and graphite.
  • the first heating furnace 122 has a metal inlet 128 for introducing metal into the first heating furnace 122.
  • a gas containing chlorine used for chlorination may be introduced into the first heating furnace 122 using the metal inlet 128.
  • a gas introduction port (third gas introduction port) 130 may be provided as an arbitrary configuration, and a gas containing chlorine may be introduced through the valve 132.
  • the gas containing chlorine may contain an inert gas such as nitrogen, argon or helium for diluting chlorine.
  • an inert gas and a gas containing chlorine hereinafter also referred to as a mixed gas
  • the amount of chlorine can be easily and precisely controlled.
  • the third gas inlet 130 is surrounded by the first heater 160, but the third gas inlet 130 is not surrounded by the first heater 160, and the first heater 160. May be exposed from.
  • the first heating furnace 122 is heated by the first heater 160, and the metal disposed in the first heating furnace 122 is chlorine gas introduced from the metal inlet 128 and / or the third gas inlet 130. Reacts with to give metal chlorides.
  • the chloride exists as a gas (vapor) in the chlorination furnace 120 or takes an equilibrium state between the gas and the liquid. In the latter case, some of the chloride is in a molten state and some is present as vapor. Molten chloride and chloride vapor generated in the first heating furnace 122 move to the second heating furnace 124 via the connecting portion 123 (or an opening when the partition member 126 is provided).
  • the second heating furnace 124 transports the chloride vapor generated in the first heating furnace 122 to the reduction furnace 200, and vaporizes the molten chloride when it is generated, thereby generating the chloride vapor.
  • the main function is to generate and transport this to the reduction furnace 200.
  • the second heating furnace 124 is surrounded by the second heater 162 and heated. As described above, the first heater 160 and the second heater 162 are independently controlled, and can heat the first heating furnace 122 and the second heating furnace 124 at different temperatures. The first heater 160 and the second heater 162 are driven so that the temperature of the second heating furnace 124 is higher than the temperature of the first heating furnace 122.
  • the temperatures of the first heating furnace 122 and the second heating furnace 124 so that the temperature of the second heating furnace 124 is increased by 200 to 300 ° C., molten chloride is generated and the first heating furnace 124 is heated. Even when moving from the heating furnace 122 to the second heating furnace 124, chloride can be quickly vaporized in the second heating furnace 124.
  • the second heating furnace 124 may be filled with the vaporization auxiliary material 140.
  • the vaporization auxiliary material 140 is, for example, a metal or semi-metal oxide such as quartz, alumina, or zirconia, ceramic, nitride such as boron nitride, particles or pellets containing graphite, and thereby vaporizes molten chloride.
  • a wide heating area can be provided.
  • the second heating furnace 124 has a discharge port 134 for transporting the vapor of chloride generated in the first heating furnace 122 or the second heating furnace 124 to the reduction furnace 200. Furthermore, a gas inlet (first gas inlet) for introducing a gas containing chlorine into the chlorination furnace 120, more specifically, at least one of the first heating furnace 122 and the second heating furnace 124. ) 136 is provided.
  • the first gas inlet 136 may be disposed so as to be surrounded by either the first heater 160 or the second heater 162. In the example shown in FIG. 2, the first gas inlet 136 is provided in the second heating furnace 124 and is surrounded by the second heater 162.
  • the first gas inlet 136 is further connected to a chlorine gas source (such as a cylinder) (not shown) via a valve 138.
  • the gas containing chlorine introduced through the first gas inlet 136 may also contain an inert gas.
  • the discharge port 134 for transporting the chloride vapor to the reduction furnace 200 is arranged at a position higher than the bottom of the second heating furnace 124. This is to prevent the molten chloride from flowing into the reduction furnace 200 without being vaporized.
  • the first gas introduction port 136 When the first gas introduction port 136 is provided in the second heating furnace 124, the first gas introduction port 136 may be disposed at a position lower than the discharge port 134 (a position farther from the first heating furnace 122). it can. This is because molten chloride tends to accumulate in the lower part of the second heating furnace 124, and by introducing a gas containing chlorine from the lower part of the second heating furnace 124, the chloride gas is efficiently supplied to the discharge port 134. This is because it can be introduced.
  • the gas containing chlorine introduced from the metal inlet 128, the first gas inlet 136, and the third gas inlet 130 gives a positive pressure to the chlorination furnace 120.
  • the vapor of chloride generated in the chlorination furnace 120 is introduced into the first transport pipe 112 through the discharge port 134 by this positive pressure and transported to the reduction furnace 200.
  • All or most of the chlorine introduced from the metal inlet 128 or the third gas inlet 130 is consumed by reaction with the metal.
  • the chlorine introduced from the first gas inlet 136 has a smaller contribution to the reaction with the metal and the consumption rate is lower than the chlorine introduced from the metal inlet 128 or the third gas inlet 130. Therefore, the chloride vapor is transported to the reduction furnace 200 in contact with chlorine added through at least the first gas inlet 136.
  • the chloride transported to the reduction furnace 200 is reduced in the reduction furnace 200 to give metal powder.
  • the obtained metal powder is further transported to the separation device 300 for purification and further isolated by a recovery device.
  • a gas containing chlorine is introduced through the metal inlet 128 and the third gas inlet 130. This gas is introduced to salify the metal and to provide a positive pressure for transporting the generated chloride vapor to the second furnace 124.
  • a gas containing chlorine is further introduced into the second heating furnace 124 through the first gas inlet 136, and a positive pressure is applied to the chlorination furnace 120. Accordingly, the chloride vapor can be efficiently sent to the discharge port 134 and the chloride vapor can be quickly transported to the reduction furnace 200. As a result, it is possible to suppress a problem that chloride remains in the second heating furnace 124 or that the chloride solidifies and precipitates in the second heating furnace 124 and the first transport pipe 112. Further, the reducing gas introduced into the reduction furnace 200 through the sixth gas inlet 206 can be prevented from flowing back through the first transport pipe 112 at the same time. For this reason, it is possible to prevent a problem that the chloride is reduced in the first transport pipe 112 and the metal is deposited to clog or damage the first transport pipe 112.
  • the gas containing chlorine introduced through the first gas inlet 136 simply gives positive pressure for introducing the vapor of chloride into the reduction furnace 200 through the outlet 134 as described above. It functions not only as a physical means but also as a chemical means for more effectively preventing the occurrence of a malfunction of the system 100 as described below.
  • the metal and chloride exist in an equilibrium state represented by the following formula.
  • gaseous chloride can be prevented from depositing as a metal by introducing chlorine gas into this equilibrium system and shifting the equilibrium to the right side (chloride side). That is, the chlorine introduced through the first gas inlet 136 is hardly consumed by the chlorination of the metal introduced into the first heating furnace 122, and therefore the second heating furnace 124 and the first transport. It can be in contact with chloride vapor in the tube 112. Therefore, chlorine introduced through the first gas inlet 136 contributes to shifting the metal-chloride equilibrium to the chloride side as a chemical means. As a result, metal precipitates from the chloride gas in the second heating furnace 124 and the first transport pipe 112, which causes clogging and breakage of the first transport pipe 112 and destruction of the second heating furnace 124. A malfunction can be suppressed more effectively.
  • the chlorination furnace 120 may include a plurality of gas inlets for supplying a gas containing chlorine that functions as a chemical means. Chlorine gas may be supplied with an inert gas.
  • a gas introduction port (second gas introduction port) 142 for introducing a gas containing chlorine into the second heating furnace 124 is further provided.
  • the second gas inlet 142 can be disposed above the outlet 134. That is, the second gas introduction port 142 is provided so that the distance from the first heating furnace 122 to the discharge port 134 is larger than the distance from the first heating furnace 122 to the second gas introduction port 142. Can do.
  • the second gas inlet 142 is connected to a chlorine source (not shown), and supply of gas containing chlorine is controlled by a valve 144.
  • the metal chloride generator 110 has a gas inlet (fourth gas inlet) 146 for introducing a heated inert gas, and a third heater 164. Also good.
  • the fourth gas inlet 146 is provided in the first heating furnace 122 and is connected to the third heater 164 through a valve 148.
  • the third heater has a function of heating the inert gas.
  • the fourth gas inlet 146 and the third heater 164 are provided, the first gas inlet 136 and the second gas inlet 142 are not necessarily provided (see FIG. 6).
  • the system 100 can be driven efficiently by adopting this configuration, and the manufacturing cost of the system 100 can be reduced, thereby reducing the metal powder at low cost. Can be provided.
  • metal is introduced into the first heating furnace 122 through the metal inlet 128.
  • metal inlet 128 copper, silver, nickel, or the like can be used as the metal.
  • the second heating furnace 124 may be filled with the vaporization auxiliary material 140 in advance.
  • the first heating furnace 122 and the second heating furnace 124 are heated using the first heater 160 and the second heater 162, respectively.
  • the temperature of the 1st heating furnace 122 also depends on the kind of metal, it can set suitably in the range of 800 degreeC or more and 1000 degrees C or less, for example.
  • the temperature of the first heating furnace 122 By setting the temperature of the first heating furnace 122 to a temperature lower than the melting point of the metal, melting of the metal (metal pellet 114) that is a raw material can be prevented.
  • the metal reacts with chlorine to give chloride.
  • the temperature of the second heating furnace 124 may be set higher than the temperature of the first heating furnace 122. Although it depends on the type of metal, it can be set appropriately within a range of, for example, 900 ° C. or more and 1200 ° C. or less. By setting the temperature of the second heating furnace 124 to a temperature higher than the boiling point of the chloride, the chloride can be quickly vaporized.
  • a gas containing chlorine is introduced into the second heating furnace 124 through the first gas inlet 136.
  • a gas containing chlorine is introduced into the first heating furnace 122 through the metal inlet 128 and / or the third gas inlet 130.
  • the chlorine concentration in the mixed gas is 0.001 wt% or more and 20 wt% or less, Alternatively, 0.01 wt% or more and 10 wt% or less, or 0.1 wt% or more and 2 wt% or less may be used.
  • the chlorine introduced through the first gas inlet 136 and the second gas inlet 142 is included.
  • the gas composition and the total flow rate may be the same or different.
  • the flow rate of the gas containing chlorine introduced through the first gas introduction port 136 may be larger than that of the gas containing chlorine introduced through the second gas introduction port 142.
  • the amount of chlorine in the gas containing chlorine introduced into the second heating furnace 124 via the first gas inlet 136 and the second gas inlet 142 may be the metal inlet 128 and / or the third gas. It is preferable that the amount of chlorine contained in the gas containing chlorine introduced into the first heating furnace 122 through the gas inlet 130 is smaller than the amount of chlorine. Thereby, the chlorine content of the metal powder obtained can be reduced.
  • the temperature of the nitrogen gas may be, for example, 800 ° C. or more and 1000 ° C. or less.
  • Chloride vapor generated in the chlorination furnace 120 is discharged from the discharge port 134 and is introduced into the reduction furnace 200 from the fifth gas introduction port 204 via the first transport pipe 112.
  • a reducing gas selected from hydrogen, hydrazine, ammonia, methane, and the like is supplied from the sixth gas inlet 206 (see FIG. 1), and its flow rate and concentration are equal to or higher than the stoichiometric ratio that reacts with chloride. You may adjust to.
  • the metal powder generated in the reduction furnace is physically transported to a recovery device (not shown) such as a separation device 300 or a bag filter by the nitrogen gas introduced into the reduction furnace 200 and isolated.
  • the metal powder can be manufactured by the above steps.
  • the gas containing chlorine introduced into the second heating furnace 124 from the first gas inlet 136 or the second gas inlet 142 is quickly and physically used as a physical means. Not only has the function of stably transporting the chloride vapor to the reduction furnace 200, but also has the function of preventing metal deposition as a chemical means. For this reason, by applying this embodiment, it is possible to provide a metal powder production system that can be driven stably and can produce metal powder efficiently.
  • the metal chloride generator 116 has the same structure as that of the metal chloride generator 110 in that at least the first heating furnace 122 and the second heating furnace 124 have different inner diameters, and the second heating furnace 124 has a tube shape. Different.
  • the second heating furnace 124 has a tube shape, and its inner diameter is smaller than that of the first heating furnace 122.
  • chloride vapor and chlorine gas can be mixed more effectively, and the physical and chemical properties of the gas containing chlorine introduced through the first gas inlet 136 can be reduced. The effect can be increased.
  • the first gas inlet 136 is provided in the first heating furnace 122 and is surrounded by the first heater 160.
  • the first gas inlet 136 is preferably disposed so as to be closer to the second heating furnace 124 than the metal inlet 128. This is because when molten chloride is generated, the chloride accumulates in the lower portion of the first heating furnace 122 and vaporization occurs preferentially in this portion. Therefore, as shown in FIG. 7, it is preferable to dispose the vaporization auxiliary material 140 in the first heating furnace 122 so that the upper surface is located above the first gas inlet 136.
  • the pellet 114 can be disposed on the vaporization auxiliary material 140 so as to be in contact with the vaporization auxiliary material 140.
  • the first heater 160 and the second heater 162 are driven to heat the chlorination furnace 120 and a gas containing chlorine is introduced from the metal inlet 128 and / or the third gas inlet 130.
  • a reaction between the metal and chlorine gas occurs to produce chloride.
  • Chloride present as steam moves to the second heating furnace 124 through the gap between the vaporization aids 140.
  • the liquid chloride in a molten state is vaporized by absorbing the thermal energy supplied from the first heater 160 while penetrating the layer of the vaporization auxiliary material 140, and then moves to the second heating furnace 124. To do.
  • generation apparatus 116 the production
  • the gas containing chlorine introduced from the first gas inlet 136 not only introduces chloride vapor into the second furnace 124 as a physical means, but also chemically.
  • metal precipitation from chloride can be prevented.
  • the precipitation of metals and chlorides can be effectively suppressed even in the tube-shaped second heating furnace 124, and the system 100 can be stably operated without causing damage or destruction.
  • Metal powder can be provided efficiently.
  • the overall length may be increased without causing an increase in the occupied area by folding the tube-shaped second heating furnace 124.
  • the boiling point of the chloride is high, it takes a relatively long time to vaporize in the second heating furnace 124, so this configuration is particularly effective when producing a metal powder that gives a chloride having a high boiling point.
  • Example 1 In this embodiment, an example will be described in which copper powder is manufactured using a system 100 including a metal chloride generator 110 having the structure shown in FIG. 2 as a basic structure. Specifically, copper pellets were placed in the first heating furnace 122 and quartz pellets were placed in the second heating furnace 124. In this state, the first heater 160 and the second heater 162 were used to heat the first heating furnace 122 and the second heating furnace 124 to 900 ° C. and 1150 ° C., respectively. A mixed gas containing nitrogen and chlorine was introduced from the metal inlet 128 and the first gas inlet 136, respectively. The chlorine concentration of the mixed gas is as shown in Table 1.
  • Table 1 shows the flow ratio of the mixed gas introduced from the metal inlet 128 when the flow rate of the mixed gas introduced from the first gas inlet 136 is 1.0 (that is, the first gas inlet 136).
  • the flow ratio of the mixed gas introduced from the metal inlet 128 with respect to the mixed gas introduced from is also described.
  • the reaction time was 10 hours.
  • the first heater 160 and the second heater 162 were removed, and the chlorination furnace 120 was observed. As a result, it was confirmed that deposition of copper chloride was not observed in the lower part of the second heating furnace 124 and that the second heating furnace 124 was not damaged.
  • Example 2 In this embodiment, an example in which copper powder is manufactured using a system 100 including a metal chloride generator 110 having the structure shown in FIG. 4 as a basic structure will be described. Specifically, copper pellets were placed in the first heating furnace 122 and quartz pellets were placed in the second heating furnace 124. In this state, the first heater 160 and the second heater 162 were used to heat the first heating furnace 122 and the second heating furnace 124 to 900 ° C. and 1150 ° C., respectively. A mixed gas containing nitrogen and chlorine was introduced from each of the metal inlet 128, the first gas inlet 136, and the second gas inlet 142. The reaction was performed in two stages.
  • the chlorine concentration inside is as shown in Table 2.
  • the first gas inlet 136 and the second gas inlet 142 are connected to the same mixed gas source, and the concentration of each component of the mixed gas introduced from these gas inlets is the same.
  • the reaction times of the first stage and the second stage were 9 hours and 8 hours, respectively.
  • Example 1 After completion of the reaction at each stage, the first heater 160 and the second heater 162 were removed, and the chlorination furnace 120 was observed. As a result, compared with Example 1, it was confirmed that precipitation of metallic copper inside the chlorination furnace 120 was significantly reduced. Moreover, it was confirmed that the precipitation of copper inside the first transport pipe 112 also decreased.
  • Example 3 the influence of the chlorine concentration of the mixed gas introduced from the first gas inlet 136 was examined using the system 100 including the metal chloride generator 110 having the basic structure shown in FIG. Results are shown. Specifically, copper pellets were placed in the first heating furnace 122 and quartz pellets were placed in the second heating furnace 124. In this state, the first heater 160 and the second heater 162 were used to heat the first heating furnace 122 and the second heating furnace 124 to 900 ° C. and 1150 ° C., respectively. Both the metal inlet 128 and the first gas inlet 136 introduced a mixed gas containing nitrogen and chlorine.
  • the first heater 160 and the second heater 162 were removed, and the chlorination furnace 120 was observed.
  • a gas containing chlorine is introduced from the first gas inlet 136
  • chlorine gas was not introduced from the first gas inlet 136 (Experiment 3)
  • metal or chloride is deposited inside the chlorination furnace 120, or deposited inside the first transport pipe 112, etc. It was confirmed that the above problems can be suppressed.
  • DESCRIPTION OF SYMBOLS 100 Metal powder manufacturing system

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  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
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PCT/JP2019/013277 2018-03-30 2019-03-27 金属塩化物生成装置、および金属粉体の製造方法 WO2019189411A1 (ja)

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