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WO2022044763A1 - Dispositif de revêtement à lit fluidisé - Google Patents

Dispositif de revêtement à lit fluidisé Download PDF

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Publication number
WO2022044763A1
WO2022044763A1 PCT/JP2021/029163 JP2021029163W WO2022044763A1 WO 2022044763 A1 WO2022044763 A1 WO 2022044763A1 JP 2021029163 W JP2021029163 W JP 2021029163W WO 2022044763 A1 WO2022044763 A1 WO 2022044763A1
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WIPO (PCT)
Prior art keywords
plasma
fluidized bed
particles
gas
processing container
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/JP2021/029163
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English (en)
Japanese (ja)
Inventor
英二郎 岩瀬
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Fujifilm Corp
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Fujifilm Corp
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Filing date
Publication date
Application filed by Fujifilm Corp filed Critical Fujifilm Corp
Priority to JP2022545610A priority Critical patent/JP7463528B2/ja
Publication of WO2022044763A1 publication Critical patent/WO2022044763A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
    • B01J8/24—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles according to "fluidised-bed" technique

Definitions

  • the present invention relates to a fluidized bed coating device that applies a substance to powder using a fluidized bed.
  • a fluidized bed coating (fluidized bed drying) is known as a technique for applying some substance to the surface of particles.
  • fluidized bed coating particles to be treated are introduced into the processing container, and fluidized gas is introduced from below to form a fluidized bed in which the particles circulate in the processing vessel, and the coating liquid is sprayed on the fluidized bed. It is a technique of covering the surface of particles with a desired material by spraying.
  • Patent Document 1 describes spraying of a spray gun in a fluidized bed apparatus for granulating or coating (coating treatment) by spraying a coating liquid from a spray gun while forming a fluidized bed of particles in a processing container. It is described that the ejection pressure of air is 0.2 MPa or more and the air flow rate is 10 to 180 Nl / min. In Patent Document 1, by having such a configuration, the crushing and blowing-up phenomenon of particles due to the sprayed air flow from the spray gun is suppressed, the product quality is homogenized, the product particle size distribution is sharpened, and the product is produced. We are trying to improve the yield.
  • Such fluidized bed coating is a technique generally used in the production of pharmaceutical materials and food materials. Therefore, the particle size of the processed granules is about several hundred ⁇ m to 1 mm.
  • the conventional device for coating a fluidized bed it is possible to apply a suitable coating liquid and to coat the particles with the coating liquid as long as the particles have a particle diameter of about several hundred ⁇ m to 1 mm.
  • the particle size of the particles to be coated is a dozen ⁇ m or less, it is difficult to perform proper coating with a conventional device for coating a fluidized bed.
  • An object of the present invention is to solve such a problem of the prior art, and even when the particle size of the particles to which the coating liquid is applied is small, it is preferable to properly apply the coating liquid to coat the particles. It is an object of the present invention to provide a fluidized bed coating apparatus capable of performing the above.
  • a processing container for accommodating particles to be processed and A gas introducing means for introducing a fluidized gas for forming a fluidized bed of particles to be treated into the processing vessel from the lower side to the upper side.
  • a spray device that sprays the coating liquid to be applied to the particles to be treated from below to above in the processing container.
  • a fluidized bed coating apparatus comprising: a plasma supply means for supplying plasma in a processing container.
  • the plasma supply means supplies plasma to at least a position in the processing container where the particles to be treated forming the fluidized bed fall.
  • the plasma supply means according to [1] or [2], wherein the generated plasma is supplied from the flow path into the processing container by an air flow, and the flow path is attached to the wall surface of the processing container.
  • Fluidized bed coating device [4]
  • the processing container has a shrinking region in which the cross-sectional area gradually shrinks toward the bottom.
  • the plasma supply means has an electrode pair provided in the processing container for generating plasma, and uses a flowing gas as plasma gas to generate plasma between the electrode pairs.
  • the fluidized bed coating device according to any one of [1] to [4], wherein the electrode pair is arranged with the surface direction of the electrodes facing up and down.
  • the processing container has a shrinking region in which the cross-sectional area gradually shrinks toward the bottom.
  • the fluidized bed coating device according to any one of [1] to [8], which has a tubular body that surrounds the spray head of the spraying device and extends in the spraying direction of the coating liquid.
  • the gas introducing means introduces a fluidized gas into a processing container from an introduction portion provided around a tubular body.
  • the plasma supply means generates plasma by atmospheric pressure plasma.
  • the coating liquid can be appropriately applied to the particles to suitably coat the particles.
  • FIG. 1 is a diagram conceptually showing an example of the fluidized bed coating device of the present invention.
  • FIG. 2 is a diagram conceptually showing another example of the plasma supply device.
  • FIG. 3 is a diagram conceptually showing another example of the fluidized bed coating device of the present invention.
  • the numerical range represented by using “-” means a range including the numerical values before and after "-" as the lower limit value and the upper limit value.
  • a fluidized layer of particles is formed in the processing container by the fluidized gas introduced from the lower side to the upper side of the processing container, and the coating liquid is sprayed from the lower side to the upper side by the spray device.
  • the coating liquid is applied to the surface of the particles to coat (coat, form a film) the surface of the particles.
  • the particles particles to be treated
  • various particles can be used as long as the particles can form a fluidized bed with a fluidized gas.
  • the particles include general particles formed of known materials such as silicon, metal, polymer, and rubber.
  • the particle size of the particles to which the fluidized bed coating device of the present invention applies the coating liquid there is no limitation on the particle size (particle size) of the particles to which the fluidized bed coating device of the present invention applies the coating liquid. That is, the particle size of the particles may be any particle size that allows the fluidized bed to be formed by the fluidized gas according to the specific gravity of the particles and the like. Here, as will be described later, in the fluidized bed coating apparatus of the present invention, even fine particles having a small particle size can be suitably coated with the coating liquid to coat the particles with the coating liquid.
  • the particle size of the particles to which the fluidized bed coating apparatus of the present invention is applied is preferably 2000 ⁇ m or less, more preferably 1000 ⁇ m or less, still more preferably 300 ⁇ m or less.
  • the lower limit of the particle size of the particles to which the fluidized bed coating apparatus of the present invention is applied is not limited, but the particle size of the particles is preferably 0.1 ⁇ m or more.
  • the coating liquid applied to the particles by the fluidized bed coating apparatus of the present invention there is no limitation on the coating liquid applied to the particles by the fluidized bed coating apparatus of the present invention. That is, as the coating liquid, various liquids can be used as long as they can be sprayed by a spraying device.
  • a functional solution material forming a functional layer such as a hard coat layer, an antireflection layer and a barrier layer, a coloring material such as ink, and a raw material such as TEOS (tetramethoxysilane) are liquefied. Examples thereof include a material having a shape, and a material for forming a metal film (metal layer) such as a plating solution and a complex ink.
  • FIG. 1 conceptually shows an example of the fluidized bed coating device of the present invention.
  • FIG. 1 is a diagram conceptually showing a cross section of the fluidized bed coating device 10 in the vertical direction.
  • the fluidized bed of the particles g is formed by the flowing gas from the lower side to the upper side, and the coating liquid is sprayed from the spraying device to apply the coating liquid to the surface of the particles g. It is applied and the particles g are coated with the coating liquid.
  • the fluidized bed coating device 10 shown in FIG. 1 includes a chamber 12, a lid 14, a gas introduction unit 16 for introducing a fluid gas, a spray device 18, a tubular body 20 for accommodating the spray device 18, and a plasma supply means.
  • the fluidized bed coating device 10 of the present invention includes, for example, an ultraviolet irradiation device for accelerating the curing of the coating liquid, an inert gas introduction device, and the like, as needed. May have a member (device) of.
  • the chamber 12 is a processing container that houses the particles g to be coated with the coating liquid and forms a fluidized bed of the particles g inside.
  • the chamber 12 is a cylindrical object having an open upper and lower surface having a diameter-reduced portion that is reduced in diameter downward.
  • the chamber 12 in the illustrated example has a cylindrical portion at the upper part and a truncated cone portion at the lower part, and the truncated cone portion has a shape in which the diameter is reduced downward, and the upper and lower surfaces are open. It is a tubular body of.
  • the shape of the chamber 12 is not limited to a cylindrical shape having a reduced diameter portion whose diameter is reduced downward in the illustrated example. That is, in the present invention, the chamber is used in an apparatus for forming a fluidized bed of particles and treating the particles with a coating liquid (coating), heat treatment, granulation, denaturation (transformation), and the like.
  • Various shapes of chambers (processing containers) are available. In the following description, a device that forms a fluidized bed of particles and processes the particles is also referred to as a "fluidized bed device" for convenience.
  • Examples of the shape of the chamber 12 include a straight tube cylinder, a downwardly reduced diameter cone, a downwardly reduced diameter truncated cone, and a combination of two or more of these. Illustrated.
  • the chamber 12 is not limited to a cylindrical shape, and may be a square cylinder shape such as a square cylinder whose cross-sectional area decreases downward, but is usually cylindrical.
  • the chamber 12 has a reduced diameter portion (reduced region) whose diameter is reduced downward as shown in the illustrated example. Further, in the chamber 12, it is preferable that the lower end of the reduced diameter portion is the lower end, that is, the bottom portion of the chamber 12. Since the chamber 12 has a reduced diameter portion whose diameter is reduced downward, it is preferable in that a fluidized bed of the particles g can be smoothly formed, and the treatment of the particles g by plasma, which will be described later, can be efficiently performed. ..
  • the material for forming the chamber 12 is not limited, and various materials used for the chamber of the fluidized bed device can be used.
  • the chamber forming material include metal materials such as stainless steel, iron and aluminum, resin materials such as acrylic resin, vinyl chloride resin and polytetrafluoroethylene, glass, and vitreous materials such as quartz. Ru.
  • the size of the chamber 12 is not limited and may be appropriately set according to the processing capacity required for the fluidized bed coating device 10.
  • the chamber 12 has a cylindrical shape having a diameter-reduced portion that is gradually reduced in diameter at the lower portion with the upper and lower surfaces open.
  • the upper surface of the chamber 12 is closed by the lid 14.
  • the lid 14 has a disk shape having a shape corresponding to the upper surface of the chamber 12, and extends downward from the lower surface to provide a cylindrical exhaust stack 14a.
  • the device of the illustrated example has two exhaust pipes 14a as an example. However, the number of exhaust stacks 14a is not limited to two, and may be one or three or more as long as sufficient exhaust is possible.
  • the exhaust stack 14a is for exhausting the fluidized gas introduced into the chamber 12 in order to form the fluidized bed of the particles g.
  • the exhaust stack 14a is covered with a filter 26.
  • the filter 26 is a filter that captures particles g that are about to escape from the exhaust stack 14a to the exhaust path 30 described later.
  • the filter 26 is not limited, and various filters used for exhausting the fluidized gas can be used in the fluidized bed apparatus.
  • the exhaust path 30 is for exhausting the fluidized gas discharged from the exhaust stack 14a to the outside of the fluidized bed coating device 10 by a predetermined route.
  • the exhaust path 30 may be a known one provided in the fluidized bed device.
  • the exhaust path of the illustrated example includes an exhaust pipe 30b connected to a region 30a covering the upper surface of the lid 14, a dust collector 30c provided in the middle of the exhaust pipe 30b, a blower provided at the end of the exhaust pipe 30b, and the like. Has an exhaust means (not shown).
  • the flow gas exhausted from the exhaust pipe 14a (fluidized bed coating device 10) of the lid 14 is exhausted to the exhaust pipe 30b from the region 30a covering the upper surface of the lid 14, and is exhausted to the exhaust pipe 30b by the dust collector 30c provided in the middle of the exhaust pipe 30b. Foreign matter such as dust is removed.
  • the fluid gas from which the foreign matter has been removed is released into the atmosphere, for example, or is supplied to a processing device for cleaning.
  • the chamber 12 has a cylindrical shape having a diameter-reduced portion that is gradually reduced in diameter with the upper and lower surfaces open.
  • the lower end of the chamber 12, that is, the open portion (opening) on the bottom surface communicates with the gas introduction portion 16.
  • a tubular body 20 is provided in the gas introduction portion 16, and a spray device 18 is housed in the tubular body 20.
  • the gas introduction unit 16 introduces the flowing gas from the bottom of the chamber 12 from the lower side to the upper side.
  • the fluidized bed coating device 10 blows particles g from below to above by the fluidized gas introduced by the gas introduction unit 16 to form a fluidized bed of particles g.
  • the gas introduction unit 16 includes a gas introduction pipe 34, a blower pipe 36, and a blower means 38.
  • the gas introduction pipe 34 is a cylindrical pipe that communicates with the opening at the bottom of the chamber 12 and coincides with the cylindrical chamber 12 in the center line.
  • the gas introduction pipe 34 is provided so as to communicate with the opening at the bottom of the chamber 12 without a gap.
  • Such a gas introduction pipe 34 introduces a flowing gas in parallel (substantially parallel) with the center line of the chamber 12.
  • the cylindrical chamber 12 is usually installed so that the center line coincides with the vertical direction. Therefore, the gas introduction pipe 34 introduces the flowing gas so as to be blown up from the lower side in the vertical direction.
  • the direction in which the flowing gas is introduced by the gas introduction unit 16, that is, the gas introduction pipe 34 is not limited to the direction parallel to the center line of the chamber 12. That is, the gas introduction pipe 34 may have an angle with respect to the center line of the chamber 12 to introduce the flowing gas.
  • the formation of the fluidized bed by the particles g can be smoothly performed, a uniform fluidized bed can be formed in the chamber 12, and the influence of the fluidized gas on the fall of the particles g in the chamber 12, which will be described later, can be further reduced.
  • the introduction direction of the fluidized gas by the gas introduction pipe 34 is preferably parallel to the center line of the chamber 12.
  • a mesh-shaped saucer 40 is provided in the middle of the gas introduction pipe 34 to prevent the particles g from falling into the gas introduction pipe 34.
  • the saucer 40 various types of trays 40 that are used as a saucer (mesh) for preventing particles from dropping unnecessarily in the fluidized bed introduction pipe can be used in the fluidized bed device.
  • blowing means 38 various blowing means used for supplying the flowing gas in a fluidized bed device such as a blower such as a blower and a compressor, a gas cylinder, a gas tank, and a cold evaporator can be used.
  • a blower such as a blower and a compressor
  • a gas cylinder such as a gas cylinder
  • a gas tank such as a gas tank
  • a cold evaporator can be used as the fluidized bed coating device 10.
  • air is preferably used as the fluidized gas, so that a blower or the like is preferably used as the blower means 38.
  • the flowing gas blown by the blower means 38 is supplied to the gas introduction pipe 34 through the blower pipe 36, and is introduced into the chamber 12 so as to be blown up from below.
  • the fluidized gas is not limited, and various gases can be used as long as they do not adversely affect the particles g and the coating liquid.
  • the fluid gas include air and an inert gas such as helium and argon.
  • air is preferably used as the fluidized gas in terms of cost, safety that can easily secure a sufficient flow rate for forming the fluidized bed, and the like.
  • the flowing gas it is preferable to use a clean gas before being supplied to the blower means 38 and / or having foreign matter removed by a filter in the blower pipe 36.
  • the flow rate of the fluidized gas the flow rate at which a desired fluidized bed can be formed may be appropriately set according to the particles g or the like to which the coating liquid is applied.
  • a circular tubular body 20 is provided so as to extend from the blower pipe 36 to the gas introduction pipe 34 and further to the inside of the chamber 12.
  • the tubular body 20 coincides with the gas introduction pipe 34, that is, the chamber 12 at the center line in the region in the gas introduction pipe 34 and the chamber 12.
  • the spray device 18 for spraying the coating liquid (coating material) is arranged in a region in the tubular body 20 that coincides with the gas introduction pipe 34 and the center line.
  • the tubular body 20 bends in the blower pipe 36 on the opposite side of the blower means 38 to reach the outside of the gas introduction portion 16.
  • a supply pipe 18a for supplying the coating liquid to the spray device 18 is inserted at a position extending to the outside of the gas introduction portion 16 of the tubular body 20.
  • the spray device 18 sprays the coating liquid to be applied to the particles g from the lower side to the upper side.
  • the spray device 18 is arranged inside the tubular body 20 housed in the gas introduction pipe 34. Therefore, the fluidized gas forming the fluidized bed of the particles g is supplied into the chamber 12 from the lower side to the upper side by the gas introduction pipe 34 so as to surround the coating liquid sprayed upward by the spray device 18.
  • the cylindrical gas introduction pipe 34 is arranged so as to coincide with the center line of the cylindrical chamber 12, and the cylindrical tubular body 20 is arranged so as to coincide with the center line of the gas introduction pipe 34.
  • the spray device 18 is arranged in the tubular body 20.
  • the spraying direction of the coating liquid by the spraying device 18 is not limited, and may be any direction from the bottom to the top.
  • the spray device 18 has the same direction as the center line of the tubular body 20, that is, the center line of the gas introduction pipe 34 and the chamber 12. It is preferable to spray the coating liquid from the bottom to the top.
  • the spray device 18 sprays the coating liquid from the lower side to the upper side so that the center line of the spray coincides with the center line of the chamber 12 or the like.
  • the particles g and the coating liquid can be more preferably mixed, and the coating liquid can be efficiently applied to the particles g.
  • the tubular body 20 is provided as a preferred embodiment. Therefore, in the fluidized bed coating device of the present invention, the spray device 18 may be provided inside the gas introduction pipe 34 so as to spray the coating liquid from below to above without having the tubular body 20. .. Alternatively, in the fluidized bed coating device of the present invention, the spray device 18 may be arranged at a position different from the gas introduction pipe 34, that is, the fluidized gas introduction pipe, and spray the coating liquid from below to above.
  • the effect of the flowing gas on the spraying of the coating liquid by the spraying device 18 that can suitably prevent clogging of the spray device 18 (spray head), that the sprayed coating liquid and the fluid gas, that is, the particles g can be suitably mixed.
  • the spray device 18 is preferably arranged in the tubular body 20 provided inside the gas introduction pipe 34 for introducing the flowing gas, as shown in the illustrated example, in terms of reduction and the like. Further, according to the configuration using the tubular body 20, since the flow gas has little influence on the spraying of the coating liquid by the spraying device 18, the spraying device 18 that does not use the fluid for spraying the droplets like the ultrasonic spray. Is also easy to use.
  • the spray device 18 preferably has a heating means for heating the coating liquid to be sprayed. Since the spray device 18 has a means for heating the coating liquid, it is preferable in that clogging of the spray head can be prevented, and even a highly viscous coating liquid can be sprayed.
  • the means for heating the coating liquid (heating method) by the spray device 18 is not limited, and various known methods can be used depending on the type and configuration of the spray device 18. Further, the coating liquid may be heated by a method such as providing a heating means in the supply pipe 18a or supplying the heated coating liquid to the supply pipe 18a. Further, the method of heating the coating liquid may be used in combination with the heating of the coating liquid by the heating means of the spray device 18.
  • the spray method (spray method) in the spray device 18 is not limited, and various known spray methods (spray coating means, spray nozzles) can be used.
  • various known spray methods such as a one-fluid spray method, a two-fluid spray method, an ultrasonic spray method, a capacitance spray method, and a centrifugal spray method can be used as the spray method.
  • the fluidized bed coating apparatus of the present invention can suitably coat fine particles g by applying a coating liquid.
  • the coating liquid is applied to such fine particles g and coated, instead of applying the entire amount of the coating liquid at once, the coating liquid is applied to the particles g little by little and the coating is applied little by little. It is preferable to do it. Therefore, it is preferable that the droplets sprayed by the spray device 18 are small.
  • the ultrasonic spray method capable of spraying fine droplets is suitably used for the fluidized bed coating device 10 of the present invention, and the ultrasonic spray method is for adjusting the droplet size. It is also suitable in terms of high degree of freedom and easy temperature control of the coating liquid.
  • a plasma supply means 24 is provided in the reduced diameter portion of the chamber 12.
  • the plasma supply means 24 of the illustrated example has a plasma generation unit 24a and a plasma supply pipe 24b.
  • the plasma generation unit 24a is a known plasma generation means having an electrode pair, a power source for applying a plasma excitation voltage to the electrode pair, and a supply means for supplying plasma gas (plasma generation gas) between the electrode pairs.
  • the plasma supply pipe 24b is a flow path (pipeline) that supplies the plasma generated by the plasma generation unit 24a into the chamber 12 by, for example, an air flow (gas flow) by plasma gas.
  • the plasma supply means 24 supplies plasma to the inside of the chamber 12 by a so-called remote plasma in which the plasma generation unit and the position where the plasma is processed are different. Further, the pressure in the chamber 12 in which the fluidized gas is introduced to form the fluidized bed of the particles g is usually atmospheric pressure. Therefore, the plasma supply means 24 needs to be an atmospheric pressure plasma, and is preferably an atmospheric pressure remote plasma capable of irradiating a remote portion separated from the plasma generating portion.
  • the chamber 12 preferably has a reduced diameter portion at the lower portion, which is reduced in diameter downward.
  • the plasma supply pipe 24b which is a flow path in the plasma supply means 24, is attached to a reduced diameter portion where the diameter below the chamber 12 is reduced. That is, the plasma supply means 24 supplies plasma to the vicinity of the inner wall surface of the chamber 12 in the reduced diameter portion.
  • the fluidized bed coating apparatus of the present invention may have three plasma supply means 24 (plasma supply pipe 24b) in the circumferential direction of the cylindrical chamber 12 at an angular interval of 120 °, or It may have four at 90 ° angular intervals, six at 60 ° angular intervals, eight at 45 ° intervals, or more. You may have the plasma supply means 24 of the above.
  • the plasma supply means 24 is not limited to being arranged at equal intervals in the circumferential direction of the chamber 12.
  • the plasma supply means 24 is provided at equal intervals in the circumferential direction of the chamber 12 in that the coating liquid can be uniformly applied to the entire particles g. Further, it is advantageous that the number of plasma supply means 24 is large. Specifically, it is preferable to provide 2 to 16 plasma supply means 24 at equal angular intervals in the circumferential direction of the chamber 12. Further, the arrangement positions of the plasma supply means 24 may be different positions in the center line direction of the chamber 12. For example, the plasma supply means 24 may be provided at two positions in the center line direction so as to be located in a zigzag manner in the circumferential direction. The above points are the same for the plasma supply means 50 (see FIG. 2) and the direct plasma (see FIG. 3), which will be described later.
  • the chamber 12 is cylindrical and has a reduced diameter portion at the lower portion that is reduced in diameter downward.
  • a gas introduction pipe 34 for introducing a fluidized gas for forming a fluidized bed of particles g is provided.
  • a tubular body 20 is provided in the gas introduction pipe 34, and a spray device 18 is arranged in the tubular body 20.
  • the gas introduction pipe 34 is provided with a saucer 40 for preventing the particles g from falling.
  • the chamber 12, the gas inlet pipe 34 and the tubular body 20 are provided center-aligned.
  • the cylindrical chamber 12 is usually arranged with its center line aligned with the vertical direction.
  • the flowing gas supplied from such a gas introduction pipe 34 is supplied from below to above in parallel (substantially parallel) with the center line in the central portion of the chamber 12. Therefore, the particles g housed in the chamber 12 are blown up by the fluidized gas from the lower center in the chamber 12 and upward in the central portion in the chamber 12, as conceptually shown by the broken line arrow in FIG. Toward, it spreads outward in the region where the momentum of the fluidized gas is reduced, descends, returns to the lower part of the center in the chamber 12, and is repeatedly blown up to form a fluidized bed.
  • a tubular body 20 is provided in the gas introduction pipe 34 so as to coincide with the center line of the gas introduction pipe 34.
  • the spray device 18 is arranged in the tubular body 20 so that the center line of the spray coincides with the center line of the tubular body 20 and the coating liquid is sprayed from the lower side to the upper side.
  • the coating liquid and the particles g are in the gas flow of the fluidized gas in the region where the flow velocity is the fastest. It gets on and is sprayed upward. Therefore, both the coating liquid and the particles g are rapidly diffused in the fluid gas and are preferably mixed.
  • the coating liquid can be uniformly applied to each particle g without causing a positional deviation in the flowing gas.
  • the application of the coating liquid to the particles g first rises from the lower center of the chamber 12, spreads outward, descends and returns to the lower center of the chamber 12, in the flow of particles shown by the broken line in FIG. Will be done. That is, due to the synergistic effect of the flow rate of the flowing gas at the coating position and the length of the flow length until recoating after coating, the particles g are dried at the time when the coating liquid is applied. is doing.
  • the fluidized bed coating device 10 of the illustrated example has a tubular body 20 in the gas introduction pipe 34, and the spray device 18 is arranged in the tubular body 20 as a preferred embodiment. Therefore, the spraying of the coating liquid by the spraying device 18 is not affected by the flowing gas. Further, since the spray of the coating liquid by the spray device 18 is not affected by the flowing gas, it is not necessary to increase the force of the spray, and the droplets can be made fine. As a result, the amount of the coating liquid applied to the particles g can be reduced to a small amount, and the coating liquid can be gradually applied to the particles g that are circulated by forming the fluidized bed. As a result, even fine particles g can be suitably coated with the coating liquid and uniformly and appropriately coated with the coating liquid.
  • the flowing gas is introduced upward from the lower center of the chamber 12 and is exhausted to the outside of the chamber 12 from the exhaust pipe 14a of the lid 14 that closes the upper surface of the chamber 12. Therefore, the flow path of the flowing gas in the chamber 12 is basically one direction from the lower side to the upper side of the chamber 12. That is, in the fluidized bed of the particles g in the chamber 12, the descent of the particles g is a drop due to its own weight, which is hardly affected by the fluidized gas, that is, the air flow.
  • the plasma supply pipe 24b of the plasma supply means 24 is attached to the wall surface of the reduced diameter portion at the lower part of the chamber 12, and the plasma P by the atmospheric pressure remote plasma is supplied into the chamber 12. ing. That is, the particles g forming the fluidized bed are preferably treated with the plasma P supplied from the plasma supply means 24 when descending.
  • the fluidized bed coating device 10 of the present invention has such a configuration, so that even fine particles g can be suitably applied and coated with the coating liquid.
  • the adhesion and covering property of the coating liquid or the like to the object to be treated can be improved.
  • surface modification by plasma treatment of the particles is effective.
  • high frequency thermal plasma treatment is known. This plasma treatment can be performed at 3000 to 15000 ° C., but it is necessary to use an inert gas as the plasma gas. It is also possible to integrate the fluidized bed and the high-frequency thermal plasma processing means and fill the entire processing container with an inert gas. However, a large-scale gas supply device is required, and the running cost is very high, which is not realistic. Further, the particles g are not necessarily resistant to heat. In consideration of the above points, in the plasma treatment of the particles g in the fluidized bed, it is preferable to use an atmospheric pressure plasma capable of treating at a low temperature.
  • the plasma treatment of the particles g forming the fluidized bed and the coating of the coating liquid on the particles g are performed in the same system. That is, even if the particles g can be uniformly treated by the atmospheric pressure plasma, instability such as surface deactivation occurs when the treatment system moves sequentially. Particle g, particularly fine particle g, has a large surface area and accelerates surface deactivation. Therefore, in the treatment of the particles g, the fact that the coating of the coating liquid and the plasma treatment are in the same system greatly leads to the application of the coating liquid to the particles g and the stability of the coating.
  • the fluidized bed coating device 10 having the plasma supply means 24 for supplying the plasma P by the atmospheric pressure remote plasma in the chamber 12, the atmospheric pressure plasma is used and the coating liquid to the particles g in the chamber 12 is used. And plasma treatment of the particles g can be performed.
  • plasma P is supplied to a position where the particles g forming the fluidized bed fall to perform plasma treatment.
  • the fluidized bed coating device 10 enables plasma treatment of more suitable particles g and coating of the coating liquid on the more suitable particles g.
  • the plasma treatment of the particles g in the fluidized bed it is important to perform the plasma treatment in a state where the particles g are sufficiently flowed and dispersed. Further, when the particles g, particularly the fine particles g, are subjected to plasma treatment, it is preferable to perform the treatment in a state where the plasma is not easily affected by the air flow or the like. When the plasma is affected by the air flow, the concentration of the plasma decreases and sufficient processing cannot be performed. It is also possible to reduce the influence of airflow by increasing the intensity of plasma and generating high-density plasma. However, considering damage to the particles g, it is not preferable that the plasma is too strong, especially for fine particles g.
  • plasma P is supplied to a position where the particles g forming the fluidized bed fall to perform plasma treatment.
  • the fluidized gas forming the fluidized bed basically passes through the chamber 12 from the lower side to the upper side. Therefore, the particles g falling in the chamber 12 fall by their own weight without being affected by the flowing gas. Therefore, by supplying the plasma P to the position where the particles g fall and performing the plasma treatment, sufficient plasma treatment of the particles g can be performed even with a gentle plasma P without being affected by the air flow.
  • the spray of the coating liquid rises from the lower center of the chamber 12, spreads outward, and descends to return to the lower center of the chamber 12.
  • FIG. It is performed first in the flow of particles shown by the broken line.
  • the droplets of the coating liquid sprayed by the spray device 18 can be made sufficiently small, and the coating liquid can be gradually applied to the particles g. Therefore, in the falling particles g, the applied coating liquid is sufficiently dried.
  • the particles g that form and circulate the fluidized bed can be repeatedly coated with the coating liquid, dried, and plasma-treated with the particles g and the dried coating liquid.
  • the supply position of the plasma P into the chamber 12, that is, the mounting position of the plasma supply pipe 24b is not limited to the wall surface of the reduced diameter portion of the chamber 12. That is, the mounting position of the plasma supply pipe 24b may be a wall surface corresponding to the position where the particles g fall.
  • the plasma supply pipe 24b may be attached to the wall surface of the region of the straight pipe in which the chamber 12 does not shrink in diameter, as long as it corresponds to the position where the particles g fall. ..
  • the mounting position of the plasma supply pipe 24b is not preferable in the vicinity of the bottom and the bottom where the flow of the particles g becomes extremely small or the air flow starts to wind up.
  • the particles g treated by the plasma P descend along the wall surface of the chamber 12, return to the lower center in the chamber 12 again, and are repeatedly blown up.
  • the coating liquid is gradually applied to the particles g, that is, the particles g are gradually coated with the coating liquid and coated.
  • the fluidized bed coating apparatus 10 of the present invention for example, it is possible to form a very thin film having a particle size of 10 ⁇ m or less on a particle having a particle size of 100 nm or less.
  • the plasma supply means 24 supplies plasma to the chamber 12 by a so-called atmospheric pressure remote plasma having a plasma generation unit 24a and a plasma supply pipe 24b.
  • the present invention is not limited to this. That is, various plasma supply means can be used in the fluidized bed coating device of the present invention.
  • FIG. 2 shows another example of the plasma supply means.
  • the example shown in FIG. 2 is also a type of atmospheric pressure remote plasma in which a flow path for supplying plasma into the chamber 12 is attached to the wall surface of the chamber 12.
  • the plasma supply means 50 shown in FIG. 2 has a double tube structure, and has an inner tube 52, an outer tube 54, a first electrode 56, a second electrode 58, and a power supply 60.
  • the inner tube 52 and the outer tube 54 are made of a glassy material such as quartz and a high melting point insulating material (dielectric material) such as a ceramic material such as alumina.
  • the inner pipe 52 and the outer pipe 54 are both circular pipes, and the inner pipe 52 is inserted into the outer pipe 54 so as to coincide with the center line.
  • the gap 62 between the inner tube 52 and the outer tube 54 is a supply path for the plasma gas PG and a flow path for the generated plasma P.
  • the outer tube 54 forming the flow path of the plasma P is attached to the reduced diameter portion of the chamber 12 or the like, similarly to the plasma supply tube 24b described above.
  • Both the first electrode 56 and the second electrode 58 are cylindrical electrodes having an inner diameter substantially the same as the outer diameter of the outer tube 54, and are arranged by inserting the outer tube 54.
  • the first electrode 56 and the second electrode 58 are arranged so as to be separated from each other in the center line direction of the outer tube 54 with the second electrode 58 on the chamber 12 side. Further, the first electrode 56 is grounded.
  • the second electrode 58 is connected to the power supply 60.
  • the power supply 60 is, for example, a high frequency pulse power supply, and a pulsed voltage having a predetermined frequency is applied to the second electrode 58.
  • the plasma gas PG is supplied from a supply source (not shown) to the gap 62 between the inner tube 52 and the outer tube 54.
  • a pulsed voltage is applied from the power supply 60 to the second electrode 58
  • a discharge region DA is formed between the first electrode 56 and the second electrode 58, and this discharge is plasma flowing through the discharge region DA. It acts on the gas PG to generate plasma P.
  • the generated plasma P further flows through the gap 62 by the flow of the plasma gas PG, and is supplied to the inside of the chamber 12 from the end of the double pipe composed of the inner pipe 52 and the outer pipe 54.
  • the plasma supply means 50 has a double tube structure including an inner tube 52 and an outer tube 54, and various processing gas MGs can be flowed inside the inner tube 52. That is, according to the plasma supply means 50, various treated gas MGs treated with plasma can be supplied into the chamber 12 by using the inner pipe 52 as needed. Therefore, according to the plasma supply means 50, in addition to the treatment of the particles g by the supplied plasma P, it is also possible to treat the particles g by the plasma-treated processing gas MG, if necessary.
  • a method of introducing TEOS (tetramethoxysilane) or the like as the treatment gas MG is exemplified.
  • plasma-treated TEOS forms modifying groups such as Si—OH and SiO 2 on the surface of the particles g to improve the adhesion between the coating (coating) with the coating liquid and the particles g. Can be done.
  • the plasma supply means is not limited to the atmospheric pressure remote plasma as described above.
  • an electrode pair 64 for generating plasma is provided inside the chamber 12, and for example, an atmospheric pressure plasma using a fluidized gas as a plasma gas is used in the chamber. Plasma may be generated inside the twelve.
  • a plasma excitation power source or the like (not shown) is connected to the electrode pair 64.
  • the plasma excitation power source a known one can be used.
  • air is preferably used as the fluid gas, so that the plasma gas is air at this time.
  • plasma treatment is applied to the particles g in which plasma is generated and passes between the electrodes constituting the electrode pair 64. That is, this example is a so-called direct plasma processing in which the plasma generation position and the processing position of the particles g by the plasma are equal to each other.
  • the arrangement position of the electrode pair 64 is not limited to the inclined portion of the chamber 12 in the illustrated example, and may be inside the chamber 12. However, as with the plasma supply means described above, it is preferable that the electrode pair 64 that generates plasma is provided at a position where the particles g forming the fluidized bed drop (fall by their own weight). Further, the electrodes are preferably provided with the surface direction facing up and down so that the falling particles g can preferably pass between the electrodes forming the electrode pair, and the surface direction is parallel to the wall surface of the chamber 12. It is more preferable to be provided. Further, for the same reason as the above-mentioned plasma supply means 24, it is more preferable that the reduced diameter portion of the chamber 12 is provided with the surface direction of the electrode parallel to the wall surface of the chamber 12, as shown in the illustrated example.
  • the electrode pair 64 for plasma generation may have a truncated cone shape corresponding to the entire circumference of the reduced diameter portion, or may be divided and arranged at equal angular intervals as in the plasma supply means 24 described above. You may. Further, in the fluidized bed coating apparatus of the present invention, the above-mentioned remote plasma and such a direct plasma may be used in combination as the plasma supply means.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Combustion & Propulsion (AREA)
  • Glanulating (AREA)
  • Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
  • Plasma Technology (AREA)
  • Special Spraying Apparatus (AREA)
  • Coating Apparatus (AREA)

Abstract

La présente invention aborde le problème de la fourniture d'un dispositif de revêtement à lit fluidisé qui peut appliquer correctement un liquide de revêtement pour effectuer un revêtement de particules, etc, même dans un cas où le diamètre de particule des particules à revêtir avec le liquide de revêtement est faible. Ce problème est résolu grâce à la présente invention comprenant : un récipient qui reçoit des particules à traiter ; un moyen d'introduction de gaz pour introduire vers le haut un gaz de fluidisation pour former un lit fluidisé pour les particules à traiter ; un dispositif de pulvérisation qui pulvérise vers le haut un liquide de revêtement qui recouvre les particules à traiter dans le récipient ; et un moyen d'alimentation en plasma pour fournir du plasma à l'intérieur du récipient.
PCT/JP2021/029163 2020-08-31 2021-08-05 Dispositif de revêtement à lit fluidisé Ceased WO2022044763A1 (fr)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2025070563A1 (fr) * 2023-09-27 2025-04-03 富士フイルム株式会社 Procédé de fabrication de cellule solaire

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH06228739A (ja) * 1993-02-02 1994-08-16 Sachiko Okazaki 大気圧プラズマによる粉体の表面処理方法とその装置
JP2003001090A (ja) * 2001-06-22 2003-01-07 Pauretsuku:Kk 流動層装置
JP2003525726A (ja) * 1999-11-22 2003-09-02 グラット プロセス テクノロジー ゲーエムベーハー 粒子を被覆する装置
JP2005523142A (ja) * 2002-04-10 2005-08-04 ダウ・コーニング・アイルランド・リミテッド 保護コーティング組成物
WO2006068165A1 (fr) * 2004-12-21 2006-06-29 Eisai R & D Management Co., Ltd. Dispositif de lit fluidise
JP2008229603A (ja) * 2007-02-22 2008-10-02 Teruhisa Hasegawa 流動層装置
JP2016182552A (ja) * 2015-03-26 2016-10-20 株式会社豊田自動織機 コート粒子製造装置

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH06228739A (ja) * 1993-02-02 1994-08-16 Sachiko Okazaki 大気圧プラズマによる粉体の表面処理方法とその装置
JP2003525726A (ja) * 1999-11-22 2003-09-02 グラット プロセス テクノロジー ゲーエムベーハー 粒子を被覆する装置
JP2003001090A (ja) * 2001-06-22 2003-01-07 Pauretsuku:Kk 流動層装置
JP2005523142A (ja) * 2002-04-10 2005-08-04 ダウ・コーニング・アイルランド・リミテッド 保護コーティング組成物
WO2006068165A1 (fr) * 2004-12-21 2006-06-29 Eisai R & D Management Co., Ltd. Dispositif de lit fluidise
JP2008229603A (ja) * 2007-02-22 2008-10-02 Teruhisa Hasegawa 流動層装置
JP2016182552A (ja) * 2015-03-26 2016-10-20 株式会社豊田自動織機 コート粒子製造装置

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2025070563A1 (fr) * 2023-09-27 2025-04-03 富士フイルム株式会社 Procédé de fabrication de cellule solaire

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