JP6281077B2 - Method and apparatus for producing fine powder - Google Patents

Description

In the present invention, a raw material to be pulverized is suspended in a liquefied inert gas such as liquid nitrogen, and this is pulverized by a medium pulverization method at an ultra-low temperature to produce a fine powder finely pulverized to submicron size or nano size. The present invention relates to a fine powder manufacturing method and a manufacturing apparatus.

The present invention also comprises two or more kinds of raw materials to be pulverized in a liquefied inert gas by a medium pulverization method and / or dispersed treatment and uniformly mixed. The present invention relates to a fine powder production method and a production apparatus capable of producing a fine powder.

  Conventionally, as a fine powder production apparatus, a dry pulverization apparatus represented by a jet mill or a hammer mill, or a wet medium pulverization apparatus such as a ball mill, a sand mill, or a bead mill has been used. In general, it is said that the wet-medium pulverizer can make the material to be pulverized finer than the dry pulverizer. Japanese Patent Laid-Open No. 5-220373 discloses a wet disperser using a composite ceramic member. Japanese Patent Application Laid-Open No. 2012-45456 discloses a wet-medium stirring and dispersing machine.

  A bead mill, which is widely used as a wet-medium pulverizer, generates a suspension (slurry) by stirring a solvent composed of water or an organic solvent and a raw material to be pulverized with a premixer. The material to be crushed is pulverized by, for example, colliding with a large number of beads (solid pulverization medium) composed of spheres having a diameter of about a few microns to several millimeters (solid pulverization medium) and colliding with the numerous beads moving in the slurry. In this apparatus, the aggregated secondary particles are dispersed to recover a liquid containing finely divided particles of the material to be crushed. Ceramic beads made of zirconia, which is chemically stable and high in hardness, or resin beads made of urethane, nylon, etc. with less metal contamination, and stainless steel Made metal beads are used.

  The fine powder of the material to be crushed generated by the bead mill is mixed with the beads for pulverization or dispersion in the suspension stored in the pulverization container of the bead mill. Usually, the beads are first separated from the suspension and then the fine powder is separated. Since the fine powder separated from the suspension is in the form of a slurry, it is necessary to obtain a dry powder through a drying process. When the powder heated in the drying process is re-agglomerated, it is necessary to pulverize or disperse again. In order to pulverize other raw materials to be pulverized using the same wet medium pulverizer, the suspension and beads are taken out from the pulverization container, and the pulverization container is washed. The washing operation of the pulverizer and the taken out beads are washed. Japanese Unexamined Patent Publication No. 2007-268403 discloses a bead mill in which the slurry remaining in the pulverizer is reduced as much as possible to facilitate maintenance of the bead mill, and the remaining slurry and micro beads can be taken out completely and easily in a short time. Is disclosed.

  The beads, which are solid grinding media of the bead mill, collide with the inner wall of the grinding container, the grinding disk, and the rotating shaft during grinding of the raw material to be ground, and generate frictional heat. At the same time, frictional heat is generated by the collision and friction between the beads and the raw material to be ground, and also by the collision and friction between the beads, and the temperature of the suspension rises. Therefore, a pulverization container cooling device is required when pulverizing raw materials that are weak against heat. Moreover, when pulverizing the material to be ground having water decomposability, it is necessary to use a medium other than water. When an organic solvent is used as a medium when it is desired to obtain a recovered product as a dry powder by wet pulverization, a slurry drying device is required, and an organic solvent recovery device is required.

  Japanese Patent Laid-Open No. 2003-1129 discloses a method in which a dry fine powder efficiently pulverized by a small-scale machine is obtained by using a medium stirring mill to suspend a suspension in which a material to be pulverized is dispersed in a liquefied inert gas. A method for producing a fine powder is proposed, characterized in that a pulverized inert gas is vaporized to obtain a dry powder. In addition, International Publication No. WO 2011/059074 discloses that a suspension of a raw material to be pulverized is generated using a liquefied inert gas as a dispersion medium, and this suspension is stirred together with beads for pulverization or dispersion by a pulverizer. Therefore, when the raw material to be pulverized is pulverized, use of beads whose particle size is in a specific range, use of granular dry ice instead of all or a part of beads for pulverization or dispersion, etc. are proposed.

Japanese Patent Laid-Open No. 5-220373 JP 2012-45456 A JP 2007-268403 A JP 2003-1129 A International Publication Number WO 2011/059074

The object of the present invention is to enable one or two or more kinds of raw materials to be continuously pulverized in a liquefied inert gas, thereby producing a fine powder of uniform quality. The object is to provide a method for producing a powder.

Another object of the present invention makes it possible to grind processing or distributed processing sequentially one or two or more of the crushed material in the liquefied inert gas by media milling process, thereby uniform powder quality An object of the present invention is to provide a fine powder production apparatus capable of producing

The fine powder production method of the present invention comprises a fine powder of the material to be crushed by pulverizing a suspension containing a liquefied inert gas and the material to be crushed by a medium pulverization method in a pulverization vessel. In the powder manufacturing method, during the pulverization treatment of the material to be pulverized , the suspension is communicated with the pulverization chamber so that the suspension can freely flow between the pulverization chamber and the pulverization chamber. indoor grinding media is partitioned from the grinding chamber so as not to flow into the service chamber, and detects the liquid surface of the suspension, the lower limit of the liquid level of the suspension in the service chamber is predetermined Upon reaching the value, if said service chamber automatically start supplying the liquefied inert gas, reaches the upper limit liquid level of the suspension in the service chamber is predetermined to said service chamber By automatically stopping the supply of liquefied inert gas, The liquid level of the suspension of the grinding vessel in the grinding process is maintained within a predetermined range, the top of the grinding vessel as liquefied inert gas vaporized in the grinding chamber to flow into said service chamber The pressure of the liquefied inert gas vaporized during the pulverization process of the raw material to be pulverized is maintained in a predetermined range in the service room defined as follows.
The apparatus for producing fine powder according to the present invention comprises a fine powder of the raw material to be pulverized by pulverizing a suspension containing the liquefied inert gas and the raw material to be pulverized by a medium pulverization method in a pulverization vessel. In the powder production apparatus, a service chamber is defined at an upper portion of a ceiling portion of the pulverization container, and a pulverization medium in the pulverization container is provided on the ceiling portion of the pulverization container during the pulverization process of the raw material to be crushed A through-hole capable of allowing the suspension to flow between the inside of the crushing container and the service chamber during the crushing process of the raw material to be crushed. forming a, to the service chamber, and the lower limit level sensor for detecting the lower limit of the suspension of the grinding vessel, and the upper limit level sensor for detecting the upper limit of the suspension of the grinding vessel, liquefied and a supply port of the inert gas, before When the lower level sensor detects the lower limit of the liquid level of the suspension, the liquefying a supply of liquefied inert gas starts from the supply port of the inert gas into the service chamber, the upper limit level sensor is the suspension When the upper limit value of the liquid level is detected, a liquid level control device is provided to stop the supply of the liquefied inert gas from the liquefied inert gas supply port to the service chamber, and the material to be crushed is provided in the service chamber. A depressurization / exhaust device is provided for discharging the liquefied inert gas vaporized during the pulverization process from the service chamber .
In the fine powder production apparatus of the present invention, the pulverization container is a pulverization container of a vertical bead mill, and an agitation disk attached to a rotating shaft of the vertical bead mill agitates the pulverization medium in the pulverization container. The pulverization medium is arranged inside the pulverization container so as to move from the peripheral edge of the ceiling part toward the rotation axis along the ceiling member of the pulverization container .

In this onset bright, it is possible to configure the pulverizng device in vertical-type bead mill. Then, the ceiling of the grinding container a vertical bead mill is passed through the rotation axis of a vertical bead mill, beads are longitudinal bead mill grinding media, are agitated in the grinding chamber of the internal powder 砕容unit, ceiling Ibe along to move toward the periphery or al rotation axis of the top Ibe, placing a vertical plurality of disks is a stirring member of bead mill grinding chamber powder砕容device is desirable.

This onset Ming, also a hollow member disposed in powdered砕容device, define a service chamber on top of the top Ibe powder 砕容device by this hollow member, grinding suspension inside the grinding container to flow between the chamber and the service chamber, it is possible to form the through hole in the ceiling Ibe. At this time, the liquid level control device, the suspension liquid level of the service chamber, for detecting whether within the control range determined in advance, and the upper level sensor and the lower limit level sensor, liquefied non a source of inert gas, a pump for pumping a liquefied inert gas supply port opened in the service chamber, the liquefied inert gas supply source or al liquefaction inert gas supply port of the liquefied inert gas, Sa When the suspension liquid level of the-bis chamber becomes lower than the control range, by operating the pump to supply liquefied inert gas into the service chamber, and service room suspension liquid When Mendaka is becomes high than the control range, the pump is stopped to stop the supply of the liquefied inert gas into the service chamber may have a liquefied inert gas autofeed equipment.

In this onset bright, also the middle empty member, communicates with the service chamber of the middle empty member, and the sample-bead inlet for introducing the pulverized starting material and bi chromatography's provided, heavenly powder砕容unit in Ibe, to be pulverized starting material and bi chromatography's inserted from the specimen beads inlet, so that it can be introduced into the service chamber or et powder砕容device, it is possible to form the through hole.

This onset Ming, further, medium empty member seal block mounted on, this sealing block is formed a rotary shaft through hole communicating with the service chamber, rotating shaft extending through the top Ibe powder 砕容unit penetrates the middle empty member service chamber and rotating shaft through hole can extend to the outside of the sealing block. At this time, as the liquefied inert gas is vaporized in powder砕容device and service chamber does not flow out to the outside from the rotation axis through hole, the shaft sealing member between the times the peripheral surface of the rotating shaft and the sheet Lumpur block Can be intervened . Reduced pressure and exhaust device is interposed between the shaft rotation axis in service chamber side than the sealing member and the service chamber, and has a fluid passage communicating with service chamber, a labyrinth seal, service and relief valve connected to the top of the chamber, may have a ring blower for vapor draw fluid passage La Birinsushiru.

The fine powder production apparatus of the present invention contains a suspension and pulverizes the material to be pulverized by a medium pulverization method, and the material to be pulverized is pulverized in a liquefied inert gas by the pulverizer. In addition to the liquid level control device that maintains the liquid level height of the suspension in a desired range so as to be processed, the pulverizing device or the liquefied inert gas vaporized by the liquid level control device, A decompression / exhaust device that flows out from the liquid level control device, and a recovery device that takes out the suspension that has been pulverized by the pulverizer from the pulverizer. The recovery device includes a recovery passage having an opening in the bottom surface of the powder砕容unit, a bead separator for separating suspensions or rabbi over's flowing powdered砕容device or we recovered passage, the recovered path And a valve device that opens and closes.

In the present invention, as the liquefied inert gas, liquid nitrogen, liquid helium, liquid neon, liquid argon, liquid krypton, or it can use liquid xenon.

In the present invention, as the grinding medium, zirconia, agate, quartz, titania, tungsten carbide, silicon nitride, alumina, stainless steel, soda glass, low soda glass, sodaless glass, high specific gravity glass, or solid carbon dioxide (dry ice) or can be used bead solids nitrous oxide.

When the raw material to be pulverized is pulverized in a liquefied inert gas such as liquid nitrogen, the liquid nitrogen and the like are gradually vaporized and the volume thereof is reduced. Therefore, it is necessary to replenish the pulverization container appropriately. In addition , the liquid level control device automatically replenishes the liquefied inert gas during the grinding process of the material to be ground. No need to bother the operator. Therefore, it is possible to mass-produce pulverized products of uniform quality. The term pulverization used in this specification includes not only “pulverization” in which energy is input to solid particles and the size of the particles is reduced to generate new surfaces, but also mechanical energy is applied to the aggregated particles. This includes “disintegration” in which the particles are unloaded and the solid particles are refined and spread into other substances.

The fine powder production apparatus of the present invention can also be equipped with a decompression / exhaust device that causes liquid nitrogen or the like vaporized by the pulverizer or liquid level control device to flow out of the pulverizer or liquid level control device . Thereby , rupture due to suffocation or blockage can be prevented in advance. In order to prevent the liquefied inert gas vaporized in the crushing container and the service room from flowing out of the rotary shaft through hole of the seal block, a shaft sealing member is provided between the peripheral surface of the rotary shaft of the crusher and the seal block. In addition, when a labyrinth seal is interposed between the rotating shaft closer to the service room than the shaft seal member and the service room, moisture in the air is mixed and the labyrinth seal freezes. The relief valve connected to the top of the can be opened to avoid rupture due to blockage.

In addition, during the pulverization process, a service chamber that controls the liquid level of the suspension is included, except that the pulverization container of the pulverizer is filled with volatile fluid and the fluid path of the labyrinth seal is evacuated. Thus, a closed circuit is configured. Therefore, it is possible to reduce the possibility of icing due to moisture mixed in the pulverization container and the service room. If necessary, the pulverizer and its peripheral equipment can be housed in a sealed container, and the inside of the sealed container can be filled with nitrogen gas or the like to prevent moisture in the air from entering.

  When the pulverization process is completed, the pulverized suspension can be taken out by the recovery device. When pulverization media such as zirconia beads are used for the pulverization process, the beads in the suspension are separated by a separator, so only a suspension of a solvent such as liquid nitrogen and the pulverized raw material to be pulverized is used. Can be taken out. Since a solvent such as liquid nitrogen is vaporized in the air, fine powder after pulverization can be obtained as a powder without passing through a special drying step. At this time, the fine powder of the raw material to be crushed adhering to the zirconia beads or the like can be recovered by flushing the inside of the pulverization container with a solvent such as liquid nitrogen. When dry ice beads are used for the pulverization process, the dry ice beads micronized by the pulverization process may be collected together with the suspension, but the dry ice beads sublimate at room temperature. Does not require a drying process.

Incidentally, by performing low temperature grinding process of the pulverized starting material in the liquefied inert gas such as liquids nitrogen, grinding vessel is cooled by the liquefied inert gas, cooling the grinding container is not required. It is not necessary to form a cooling water passage in the grinding container.

Other features of this onset Ming, made with reference to the drawings, will become apparent from the following description.

FIG. 1 is a schematic diagram showing an outline of the configuration of the fine powder production apparatus of the present invention. Example 1 FIG. 2 is a longitudinal sectional view of a crushing apparatus incorporated in the manufacturing apparatus of FIG. 3 shows an upper limit level sensor and a lower limit level sensor of the liquid level control device incorporated in the manufacturing apparatus of FIG. 1, and FIG. 3 (A) is a cross-sectional view showing an attachment state of the upper limit level sensor. (B) is sectional drawing which shows the attachment state of a lower limit level sensor. FIG. 4 is a plan view of the hollow member incorporated in the manufacturing apparatus of FIG. FIG. 5 is a plan view of the hollow member of FIG. 4 and a seal block attached to the hollow member.

Hereinafter, an apparatus for producing fine powder using liquid nitrogen as a liquefied inert gas and incorporating a vertical bead mill as a grinding apparatus will be described.

As shown in FIG. 1, a fine powder production apparatus 1 according to the present invention includes a vertical bead mill 2 that contains a suspension to be pulverized and pulverizes a material to be pulverized by a medium pulverization method, and a material to be pulverized. Is maintained in a desired range so that the liquid level of the suspension is pulverized in the liquefied inert gas by the vertical bead mill 2 , and the pulverization container of the vertical bead mill 2 6 or the liquefied inert gas vaporized in the service chamber 10 to which the liquid level control device 3 is connected is caused to flow out from the grinding chamber 6 of the vertical bead mill 2 or the service chamber 10 to which the liquid level control device 3 is connected. An exhaust device 4 and a recovery device 5 for taking out the suspension pulverized by the vertical bead mill 2 from the vertical bead mill 2 are provided.

In FIG. 1, reference numeral 6 is a grinding container of the vertical bead mill 2, 7 is a rotating shaft, 8 is a stirring disk, and 9 is a ceiling portion of the grinding container 6. The inside of the grinding container 6 becomes a grinding chamber. The rotating shaft 7 of the vertical bead mill 2 passes through the ceiling portion 9 of the crushing container 6 and extends to the outside, and is driven at a desired rotational speed by an electric motor (not shown). The agitation disc 8 can be a pinned disc. The stirring disk 8 is configured such that beads (not shown) that are grinding media of the vertical bead mill 2 are stirred in the grinding container 6 and directed from the peripheral edge of the ceiling portion 9 toward the rotary shaft 7 along the ceiling portion 9. So as to move in the direction of arrow Z.

As shown in FIG. 1, a service room 10 is defined in the upper part of the ceiling portion 9 of the crushing container 6. Here, a through-hole 9 b is formed in the ceiling portion 9 so that the suspension flows between the pulverization container 6 and the service chamber 10. The liquid level control device 3 includes an upper limit level sensor 11 and a lower limit level sensor 12 that detect whether the liquid level height T of the suspension in the service room 10 is within a predetermined control range Y. , A liquid nitrogen supply source LN2 container 13, a liquid nitrogen supply port 14 that opens to the service chamber 10, a pump 15 that pumps liquid nitrogen from the LN2 container 13 to the liquid nitrogen supply port 14, When the liquid level height T of the suspension becomes lower than the control range Y, by operating the pump 15 the liquid nitrogen is supplied to the service chamber 10, the liquid level height T of the suspension of the service chamber 10 When it becomes higher than the control range Y, it has the liquid nitrogen automatic supply apparatus 16 which stops the pump 15 and stops supplying liquid nitrogen to the service room 10. In FIG. 1, reference numeral 17 indicates an overflow path for discharging the suspension from the service room 10 when the liquid level control device 3 malfunctions and the liquid level height T in the service room 10 increases. . The liquid nitrogen automatic supply device 16 can use the SXDII type manufactured by MR Technology, Inc. In FIG. 1, reference numeral 14 a indicates a gas-liquid separator interposed in a system path connecting the LN2 container 13 and the liquid nitrogen supply port 14.

As shown in FIG. 1, a seal block 18 is disposed in the upper part of the service room 10, and a rotary shaft through hole 19 communicating with the service room 10 is formed in the seal block 18. The rotating shaft 7 penetrating the ceiling portion 9 of the crushing container 6 passes through the service chamber 10 and the rotating shaft through hole 19 and extends outside the seal block 18. A shaft sealing member 20 is interposed between the peripheral surface of the rotating shaft 7 and the seal block 18 so that liquid nitrogen vaporized in the crushing container 6 and the service chamber 10 does not flow out from the rotating shaft through hole 19. ing. Here, the decompression / exhaust device 4 has a ring blower 21 that draws air from the rotary shaft through hole 19 on the service chamber 10 side of the shaft seal member 20, and a relief valve 22 connected to the upper portion of the service chamber 10. Have Accordingly, in FIG. 1, reference numerals L, M, and N respectively indicate a pulverization unit, a suspension liquid level control unit, and a decompression / exhaust unit.

  Referring to FIG. 1, the recovery device 5 has a valve device 23 that opens and closes the recovery passage.

FIG. 2 is a cross-sectional view showing a more detailed structure of each device that constitutes the pulverizing part L, the suspension liquid level control part M, and the decompression / exhaust part N of FIG.
The vertical bead mill 2 constituting the pulverization part L has a cylindrical pulverization container 6, and the inside of the pulverization container 6 is a pulverization chamber. As shown in FIG. 2, the pulverization container 6 includes a zirconia inner cylinder 6a, a stainless outer cylinder 6b, and a synthetic resin intermediate layer 6c that form a liquid contact portion. The ceiling portion 9 of the crushing container 6 is configured by a zirconia ceiling member 90 having a tapered cone portion 9a protruding toward the inside of the crushing vessel 6 and a through hole 9b formed at the tip of the tapered cone portion 9a. A packing 91 is interposed between the ceiling member 90 and the crushing container 6. As packing 91, VALCALON 7020 (operating temperature range from −200 ° C. to + 200 ° C.) was used.

The bottom surface portion of the pulverization container 6 is composed of a bottom plate member 60 made of zirconia, and an opening 61 is formed in the central portion of the bottom plate member 60. A recovery passage 5a of the recovery device 5 is connected to the opening 61, and a bead separator 5b for separating beads from a suspension flowing from the pulverization container 6 into the recovery passage 5a is disposed. The valve device 23 opens and closes the collection passage 5a. The valve device 23 is made of a material that is difficult to freeze, and is, for example, a brass valve device. A packing 62 is interposed between the bottom plate member 60 and the crushing container 6. As packing 62, VALCALON 7020 (operating temperature range from −200 ° C. to + 200 ° C.) was used.

The rotating shaft 7 is made of SUS304, and four zirconia pinned disks 8 are fixed to the rotating shaft 7. A pin 8 a protrudes from the lower surface of the disk 8, and a through hole 8 b is formed in the disk 8. These discs 8 are arranged at intervals in the axial direction of the rotating shaft 7, the bead is a grinding medium of a vertical bead mill 2 (not shown.) Is stirred in the grinding chamber of the inner portion of the grinding container 6 Thus, it is arranged in the crushing chamber inside the crushing container 6 so as to move in the direction of the arrow Z from the peripheral part of the ceiling part 9 toward the rotation axis 7 along the ceiling part 9 (see FIG. 1).

The suspension liquid level control unit M shown in FIG. 2 includes a service chamber 10, which is formed on a zirconia ceiling member 90 by a zirconia hollow member 100. The service chamber 10 and the inside of the crushing container 6 communicate with each other through the through hole 9b of the ceiling member 90. The hollow member 100 is provided with a sample / bead insertion port 101 for communicating with the service chamber 10 and for introducing the material to be crushed and beads into the service chamber 10. A lid 102 is detachably attached to the sample / bead inlet 101, and the raw material to be crushed and the beads as the pulverized material are put into the service room 10 from the sample / bead inlet 101 by removing the lid 102. The When the material to be crushed and the beads are charged, the sample / bead inlet 101 is hermetically sealed by the lid 102. The pulverized starting material and beads turned the sample beads inlet 10 1 or colleagues, it falls to taper cone portion 9a of the ceiling member 90, through the annular gap between the outer peripheral surface of the rotary shaft 7 and the through-hole 9b Then, it falls into the grinding chamber inside the grinding container 6.

As shown in FIGS. 3 to 5, the hollow member 100 has an upper limit level for detecting whether or not the liquid level height T of the suspension in the service chamber 10 is within a predetermined control range Y. A sensor 11, a lower limit level sensor 12, and a liquid nitrogen supply port 14 opened to the service room 10 are provided. The functions of these devices are as described above. The suspension in the service chamber 10 flows freely between the outer peripheral surface of the rotating shaft 7 and the pulverization chamber inside the pulverization container 6 through an annular gap between the through hole 9b.

A seal block 18 is fixed on the hollow member 100. The seal block 18 is fixed to the hollow member 100 with the PTFE-impregnated grant packing 201 interposed therebetween. The PTFE impregnated grant packing 201 is paired with a labyrinth seal 200 attached to the rotating shaft 7 to define a fluid passage 202, which is between the service chamber 10 and the opening 18 a of the seal block 18. Extend. A ring blower 21 is connected to the opening 18a of the seal block 18 (see FIG. 1). As described above, the ring blower 21 forcibly evaporates the vaporized liquid nitrogen from the service room 10 and performs decompression and exhaust in the service room 10. The seal block 18 is also formed with a relief passage 18b extending between the service chamber 10 and the outer surface of the seal block 18, and a relief valve 22 is connected to the relief passage 18b (see FIG. 1). .

  As described above, the rotary shaft through hole 19 communicating with the service chamber 10 is formed in the seal block 18, and the rotary shaft 7 penetrating the ceiling portion 9 of the crushing container 6 is connected to the service chamber 10 and the rotary shaft through hole. 19 and extends outside the seal block 18 (see FIG. 2). Further, a shaft seal member 20 is interposed between the outer peripheral surface of the rotary shaft 7 and the seal block 18 so that liquid nitrogen vaporized in the pulverization container 6 and the service chamber 10 does not flow out from the rotary shaft through hole 19. It is disguised.

As is clear from the above description, according to the fine powder production apparatus of the present invention, the liquid level control device automatically replenishes the liquefied inert gas during the pulverization of the material to be crushed. If raw materials are charged, even in the case of a pulverization process for a long time, the operator's hand is not troubled until the completion. Therefore, it is possible to mass-produce uniform quality pulverized.

  In Example 1, the pulverized raw material was pulverized by stirring the zirconia beads and dry ice beads as the pulverizing medium together with the pulverized raw material in a liquefied inert gas such as liquid nitrogen. Then, without using liquid nitrogen, we propose a dry ice mill that forcibly agitates only dry ice beads as a grinding medium and the material to be ground (powder) using a bead mill, and pulverizes the material to be ground (powder). . Since dry ice sublimes at room temperature, it does not contaminate the material to be crushed. Moreover, since dry ice sublimates, the recovery rate does not decrease due to adhesion to the grinding medium. Furthermore, since dry ice is a refrigerant, heat generation during pulverization can be suppressed. And since liquids, such as liquid nitrogen, are not used, it can grind | pulverize also with a vertical dry pulverizer and a horizontal dry pulverizer. Furthermore, if necessary, a continuous dry ice mill can be provided by using a blower or a bag filter. However, since dry ice beads have a relatively weak crushing force, an automatic filling device is required. Dry ice beads are preferably stored in liquid nitrogen until they are automatically filled. If dry ice beads are filled with an appropriate amount of liquid nitrogen during the automatic filling of dry ice beads, the cooling power of liquid nitrogen reduces the heat generated during pulverization by the dry ice mill more effectively. The shape of can also be held longer.

The fine powder production method and apparatus of the present invention can produce various raw materials used for products in various fields such as pharmaceuticals, cosmetics, paints, copying machines, solar cells, secondary batteries, and recording media. .

DESCRIPTION OF SYMBOLS 1 Fine powder manufacturing apparatus 2 Vertical bead mill 3 Liquid level control apparatus 4 Pressure reduction / exhaust apparatus 5 Recovery apparatus

Claims (3)

In the method for producing a fine powder, the suspension containing the liquefied inert gas and the raw material to be pulverized is pulverized by a medium pulverization method in a pulverization vessel to produce the fine powder of the pulverized raw material. During the pulverization process, the suspension communicates with the pulverization chamber so that the suspension can freely flow between the pulverization chamber and the pulverization medium in the pulverization chamber so as not to flow. is partitioned from the grinding chamber, a service chamber, and detects the liquid surface of the suspension, the liquid level of the suspension in the service chamber reaches a predetermined lower limit value, liquefaction to the service chamber starting the supply of the inert gas automatically reaches the upper limit liquid level of the suspension is predetermined in the service chamber, automatically the supply of liquefied inert gas into said service chamber By stopping, in the grinding container during grinding process The liquid level of the serial suspension is maintained at a predetermined range, in the service chamber defined above the grinding container as liquefied inert gas vaporized in the grinding chamber to flow into said service chamber A method for producing fine powder, characterized in that the pressure of the liquefied inert gas vaporized during the pulverization treatment of the material to be pulverized is maintained within a predetermined range . In a fine powder manufacturing apparatus, a suspension containing a liquefied inert gas and a raw material to be pulverized is pulverized in a pulverization container by a medium pulverization method to produce a fine powder of the pulverized raw material . A service room is defined at the top of the ceiling, and a ceiling member is provided at the ceiling of the crushing container to prevent the crushing medium in the crushing container from flowing into the service room during the crushing process of the material to be crushed. Providing a through hole in the ceiling member that allows the suspension to flow between the pulverization container and the service chamber during the pulverization processing of the raw material to be crushed; A lower limit level sensor for detecting a lower limit value of the suspension in the pulverization container; an upper limit level sensor for detecting an upper limit value of the suspension in the pulverization container; and a liquefied inert gas supply port. The lower level sensor is the suspension. Detection when detecting the lower limit, the feed was started of the liquefied inert gas from the supply port of the liquefied inert gas into the service chamber, the upper limit value of the upper limit level sensor is a liquid level of the suspension of the liquid surface Then, a liquid level control device is provided to stop the supply of the liquefied inert gas from the supply port of the liquefied inert gas to the service chamber, and the liquefaction vaporized during the pulverization processing of the material to be crushed is provided in the service chamber. An apparatus for producing fine powder, characterized in that a depressurization / exhaust device for discharging an inert gas from the service room is provided . 3. The apparatus for producing fine powder according to claim 2, wherein the pulverization container is a pulverization container of a vertical bead mill, and an agitation disk mounted on a rotating shaft of the vertical bead mill is configured to store the pulverization medium in the pulverization container. Stirring, wherein the pulverization medium is disposed inside the pulverization container so as to move from the peripheral part of the ceiling part toward the rotation axis along the ceiling member of the pulverization container , Apparatus for producing the fine powder .

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