WO2019175954A1

WO2019175954A1 - Device for producing dry powder using spray freeze granulation and system for producing dry powder using spray freeze granulation

Info

Publication number: WO2019175954A1
Application number: PCT/JP2018/009652
Authority: WO
Inventors: 晋也川口
Original assignee: 株式会社プリス
Priority date: 2018-03-13
Filing date: 2018-03-13
Publication date: 2019-09-19
Also published as: JP7038435B2; JPWO2019175954A1

Abstract

[Problem] To provide a device for producing a dry powder using spray freeze granulation and a system for producing a dry powder using spray freeze granulation, wherein manual steps are minimized and mass production of a dry powder through continuous operation and long-term operation is possible. [Solution] Provided is a device for producing a dry powder using spray freeze granulation, the device being provided with: a spray mechanism part which has a freezing preventing means and sprays a raw liquid into a freeze granulation chamber; and a freeze drying part which is configured to be detachable from a lower part of the freeze granulation chamber, has a storage container for storing frozen granulated bodies generated inside the freeze granulation chamber, and freezes and dries the frozen granulated bodies stored inside the storage container, wherein the freeze granulation chamber is cooled by any one or a combination of direct cooling, in which cooling is performed by introducing a coolant directly into the chamber, and indirect cooling, in which cooling is performed by filling a coolant into a jacket structure provided around the freeze granulation chamber. Also, provided is a system for producing a dry powder using spray freeze granulation, wherein the system, in addition to the device for producing a dry powder, is also provided with a collection means for collecting moving frozen granulated bodies according to the discharge of the coolant.

Description

Spray freeze granulated dry powder manufacturing apparatus and spray freeze granulated dry powder manufacturing system

The present invention relates to a spray freeze granulated dry powder production apparatus and spray for producing a frozen granule by rapidly cooling a sprayed undiluted solution and producing a dry powder by freeze drying the produced frozen granule. The present invention relates to a freeze granulated dry powder production system.

In the field of manufacturing food, pharmaceuticals, agricultural chemicals, chemicals, metal materials, industrial materials, etc., it is possible to produce spherical granules with excellent fluidity, and it is possible to dry heat-sensitive materials, low density From the advantage that it is possible to produce soft granules, spraying the stock solution such as slurry and solution, rapidly cooling this to produce frozen granules, and freeze-drying the generated frozen granules Thus, a freeze granulation drying method capable of obtaining a dry powder is preferably used.

For example, Non-Patent Document 1 describes a freeze granulation drying method and a rough apparatus configuration, and discloses that a ceramic dry powder can be obtained through a series of treatments.

As shown in FIG. 12, the freeze granulation drying apparatus disclosed in Non-Patent Document 1 mixes a stock solution and a compressed gas and sprays the mixture into liquid nitrogen maintained at −196 ° C. through a nozzle. To produce frozen granules. The produced frozen granule is separately collected in a collection container such as a bat cooled in advance, and then dried by a freeze dryer.

However, in the prior art shown in FIG. 12, the evaporation of liquid nitrogen is intense, and it is necessary to periodically replenish liquid nitrogen. The risk of nozzle clogging due to icicle-shaped frozen solids adhering to the nozzle discharge port. However, when the amount of the frozen granulated material in the liquid nitrogen increases, there is a problem that the stirring with the stirring bar of the magnetic stirrer causes a problem, and it is necessary to frequently collect the frozen granulated material. All of these processes must be performed manually, and the supply of the stock solution must be stopped during the process, resulting in a problem that mass production by continuous operation is difficult. Furthermore, the frozen granulation recovered from the liquid nitrogen must be thinly laid in a collection container that has been manually cooled in advance, and then provided to the freeze dryer. If this operation is not completed quickly, Melting began and was a factor in quality degradation.

The present invention has been made in view of such a situation, and the problem of the present invention is that spray freezing granulation drying which can eliminate the manual process as much as possible, and can mass-produce dry powder by continuous operation and long-time operation. It is to provide a powder production apparatus and a spray freeze granulated dry powder production system.

In order to solve the above-mentioned problem, the spray freeze granulated dry powder manufacturing apparatus according to the present invention generates a frozen granulated body in a freezing granulation chamber by cooling a continuously supplied stock solution, A spray freeze granulation dry powder production apparatus for producing a dry powder by freeze-drying a frozen granulation body, having spraying prevention means, and spraying a stock solution into a freeze granulation chamber The mechanism and a lower part of the freezing granulation chamber are configured to be detachable, and have a storage container for storing the frozen granulation generated in the freezing granulation chamber, and the frozen granulation stored in the storage container A freeze-drying section for freeze-drying, and the freeze-granulation chamber directly cools by introducing the cooling medium directly into the chamber and cools the jacket to the jacket structure provided around the freeze-granulation chamber. Indirect cooling that cools by filling It is characterized by being cooled by any or a combination thereof.

In this case, the jacket structure may be provided with an evaporative gas input pipe for directly introducing evaporative gas obtained by evaporating the filled cooling medium into the chamber.

The storage container for storing the frozen granulated material generated in the freezing granulation chamber may be formed so as to be swingable at a predetermined angle with respect to the container longitudinal axis. It may be formed so as to be rotatable.

Further, the storage container may be formed in a shallow bottom shape in which the frozen granulation body can be left stationary, and may include a stirring member for stirring the stored frozen granulation body.

The spray mechanism unit can include any one of a two-fluid nozzle, a one-fluid pressure nozzle, an ultrasonic nozzle, and a centrifugal sprayer. It is preferable to provide an antifreeze gas supply unit for supplying a warm antifreeze gas.

By the way, as the cooling medium, liquid nitrogen, nitrogen gas obtained by evaporating liquid nitrogen, liquid argon, argon gas obtained by evaporating liquid argon, dry ice, carbon dioxide gas, cooling by cooling the atmosphere by a direct expansion type or a chiller type Gas can be used. Further, a medium remaining amount detecting means for detecting the remaining amount of the cooling medium in the jacket structure and a cooling medium replenishing means for replenishing the cooling medium in the jacket structure based on the detection result by the medium remaining amount detecting means may be provided. . The jacket structure may have a heat insulating structure.

In order to solve the above-mentioned problem, the spray freeze granulated dry powder production system according to the present invention is a freeze granulated product from a stock solution continuously supplied in a freeze granulation chamber into which a cooling medium is introduced. And a freeze freeze-dried powder production system for producing a dry powder by freeze-drying the produced freeze-granulated product, and having a freeze-preventing means, and supplying the stock solution into the freeze-granulation chamber A spray mechanism unit for spraying and a lower part of the freezing granulation chamber are configured so as to be detachable, and has a storage container for storing the frozen granulated material generated in the freezing granulation chamber, and the freezing process stored in the storage container. It is characterized by comprising a freeze-drying section for freeze-drying the granules and a collecting means for collecting the frozen granules that move as the cooling medium is exhausted.

In this case, the collecting means may include a cyclone type dust collector and / or a bag filter type dust collector.

According to the present invention, there is provided a spray freeze granulated dry powder production apparatus and a spray freeze granulated dry powder production system capable of mass production of dry powder by continuous operation and long time operation as much as possible. can do.

It is an apparatus external view explaining the apparatus structure of the spray freeze granulation dry powder manufacturing apparatus 100. FIG. 2 is a schematic diagram for schematically explaining the internal configuration of the spray mechanism section 10 and the freeze granulation chamber 30. FIG. It is the schematic explaining the structure of the centrifugal sprayer 400 which is another example of the spray mechanism with which the spray mechanism part 10 is provided. 3 is a front view illustrating the configuration of a freeze-drying unit 50. FIG. FIG. 5 is a top view illustrating the configuration of the freeze-drying unit 50 as viewed from the direction of the arrow z-axis in FIG. 4. It is a side view explaining the structure of the freeze-drying part 50 seen from the arrow y-axis direction in FIG. It is a figure explaining the modification which concerns on this invention. It is a figure explaining the modification which concerns on this invention. It is a figure explaining the modification which concerns on this invention. It is a figure explaining the modification which concerns on this invention. It is a system block diagram explaining an example of a structural example of the spray freeze granulation dry powder manufacturing system. It is explanatory drawing explaining a prior art.

Hereinafter, embodiments of the present invention will be described with reference to the drawings. In addition, this invention is not limited to the following description, In the range which does not deviate from the summary of this invention, it can change suitably.

FIG. 1A is a device external view for explaining the overall configuration of a spray freeze granulated dry powder manufacturing apparatus 100 which is a preferred example of an embodiment according to the present invention, and FIG. It is an external view of the apparatus for explaining a state where the freeze-drying unit 50 is separated from the granulating chamber 30. The spray freeze granulated dry powder production apparatus 100 includes a spray mechanism unit 10, a freeze granulation chamber 30 supported by a gantry 70 via a support member 40, and a freeze drying unit 50. The stock solution continuously supplied from the spray mechanism 10 into the freezing granulation chamber 30 is instantly frozen in the freezing granulation chamber 30 maintained at a predetermined temperature to form a frozen granulated body. The frozen granulated material naturally falls in the frozen granulation chamber 30 and is stored in a storage container in a freeze-drying unit 50 that is detachably provided at the lower portion of the frozen granulation chamber 30. When a certain amount of frozen granulated material is stored in the freeze drying unit 50, the operator separates the freeze drying unit 50 from the freeze granulation chamber 30 as shown in FIG. To obtain a dry powder. The spray freeze granulation dry powder apparatus 100 having such a configuration will be described with reference to FIGS. 2, 3, 4, 5, and 6 in addition to FIG. FIG. 2 is a schematic diagram schematically illustrating the internal configuration of the spray mechanism unit 10 and the freeze granulation chamber 30, and FIG. 3 is a centrifugal sprayer 400 which is another example of the spray mechanism provided in the spray mechanism unit 10. It is the schematic explaining the structure. 4 to 6 are a front view, a top view, and a side view for explaining the configuration of the freeze-drying unit 50. FIG. For ease of explanation and understanding, FIG. 2 will be described on the assumption that the closed structure portion of the upper part (near the top surface) of the freeze granulation chamber 30 is in an open state.

As shown in FIG. 2, in the present embodiment, an example using a two-fluid nozzle as a spray mechanism provided in the spray mechanism unit 10 will be described, but the spray mechanism applicable to the present invention is not limited to this, For example, a one-fluid pressure nozzle, an ultrasonic nozzle, a centrifugal sprayer, etc. can be used, and various circumstances such as the size and uniformity of particles obtained as a dry powder, or the physical and chemical characteristics of the stock solution to be sprayed It can be selected as appropriate in consideration.

The raw fluid supply pipe 12 and the compressed gas supply pipe 15 are connected to the two-fluid nozzle main body 11 in which the discharge part 21 for spraying the raw liquid M is formed at the tip of the freezing granulation chamber 30 side. The undiluted solution supply pipe 12 is a piping member for supplying undiluted solution M stored in the undiluted solution tank 13 to the two-fluid nozzle main body 11 via the pump 14, and the compressed gas supply tube 15 includes a compressor, a cylinder, and the like. This is a piping member for supplying compressed gas (for example, air) from the compressed gas supply unit 16 to the two-fluid nozzle body 11. The two-fluid nozzle main body 11 mixes the stock solution M supplied from these piping members and the compressed gas, and then sprays the stock solution M into the freezing granulation chamber 30 via the discharge unit 21. Further, due to the venturi effect of the compressed gas from the compressed gas supply unit 16, the stock solution M can be supplied without using the pump 14.

Note that the spray mechanism unit 10 according to the present embodiment has anti-freezing means for preventing the frozen solid material generated by freezing of the stock solution M from adhering to the discharge unit 21 of the two-fluid nozzle body unit 11. Is provided. The anti-freezing means discharges normal temperature or heated gas supplied through the gas suction filter 17, the blower blower 18, the heater 22, the HEPA filter (High Efficiency Particulate Air Filter) 19 and the like as the anti-freezing gas supply unit. An antifreeze gas pipe 20 is provided in the vicinity of the portion 21. While the stock solution M is being sprayed from the discharge part 21 of the two-fluid nozzle main body 11, generation / adhesion of icicle-shaped frozen solids is generated by room-temperature gas A such as air injected from the anti-freezing gas pipe 20. Can be suppressed, and blockage in the discharge part 21 can be prevented. Moreover, it is also possible to use pressure gas, such as a compressor and a cylinder, without using the blower blower 18.

In addition, when using a centrifugal sprayer as a spraying mechanism with which the spraying mechanism part 10 is equipped, as illustrated in FIG. 3, it is configured as a centrifugal sprayer 400 having a motor part 401, a rotating disk part 402, a stock solution supply pipe 12, and the like. can do. The rotating disk unit 402 is a member that functions as a rotating unit, and rotates at a rotational speed corresponding to the driving force applied from the motor unit 401, so that the stock solution M supplied from the stock solution supply pipe 12 is converted into the freezing granulation chamber 30. Centrifuge spray. As the rotating disk 402, for example, those having various shapes and structures such as a bell type and a pin type can be adopted.

In the present invention, as the stock solution M, various raw materials in the fields of foods, pharmaceuticals, agricultural chemicals, chemicals, metal materials, and industrial materials can be used. For example, silicon carbide, silicon nitride, aluminum nitride, zirconia Even when ceramic materials such as fine ceramic materials, glass, cement, etc., such as alumina, mullite, ferrite, forsterite, barium titanate, lead zirconate titanate, steatite, zircon are used, they are spherical and fluid. An excellent dry powder can be produced, and a dry powder suitable for an intermediate material before press molding can be provided.

2, the stock solution M sprayed from the discharge unit 21 of the two-fluid nozzle main body 11 is frozen in the freezing granulation chamber 30 to form a frozen granulated body G. The freezing granulation chamber 30 can be formed of a steel material such as stainless steel, and includes a freezing granulation chamber 31 formed in a hollow substantially cylindrical shape. A heat insulation chamber 34 is formed concentrically outwardly from the outer wall 33 of the freezing granulation chamber, and the freezing granulation chamber 31 is indirectly cooled between the outer wall 33 of the freezing granulation chamber and the inner wall 35 of the heat insulating chamber. Used as a cooling medium filling chamber 37 for charging the cooling medium, these form a jacket structure.

The freezing granulation chamber 31 is a place where the frozen granulation body G is formed from the stock solution M sprayed from the discharge part 21 of the two-fluid nozzle 11 provided in the vicinity of the top surface, and is filled in the cooling medium filling chamber 37. Due to the cooling effect of the cooling medium or the cooling medium directly introduced into the freezing granulation chamber 31, the freezing temperature at which the room temperature freezes the stock solution M (approximately −10 ° C. to −190 ° C., preferably −20 ° C. to −150 ° C.). ° C) can be maintained. In the lower part of the freezing granulation chamber 31, an opening 32 is provided so as to be able to communicate with the freeze drying unit 50 for storing the frozen granulated body G formed in the freezing granulation chamber 31. The outer wall portion around the opening portion 32 is formed with a granulation chamber side joint portion 38 using a ferrule, a band, a clamp, a flange or the like so that the freeze-drying portion 50 can be connected and communicated. .

The cooling medium filling chamber 37 provided between the freezing granulation chamber outer wall 33 and the heat insulating chamber wall 35 is filled with a cooling medium for cooling the freezing granulation chamber 31. As the cooling medium, for example, liquid nitrogen, nitrogen gas, liquid argon, argon gas, liquid helium, helium gas, dry ice, carbon dioxide gas, or the like can be used. Moreover, the cooling gas which cooled the air | atmosphere via the heat exchanger by the direct expansion type or indirect type | mold via the chiller and the refrigerator can also be used. In this case, a chiller, a refrigerator, a heat exchanger, etc. may be newly installed.

The heat insulation chamber 34 may be formed as a vacuum heat insulation structure having a double structure in which the space between the heat insulation chamber inner wall 35 and the heat insulation chamber outer wall 39 is maintained in a vacuum state, and is filled in the cooling medium filling chamber 37. Further, heat transfer from the cooling medium or outside air can be prevented. In addition, for the heat insulating chamber 34, for example, glass wool, cellulose fiber, insulation board, wool heat insulating material, heat insulating material such as rock wool, hard urethane foam, phenol foam, or vacuum heat insulating material using glass wool as a core material is used or used in combination. In addition, it is possible to devise such as mirror finishing the surface of the outer inner wall and attaching copper foil to enhance the heat insulation effect.

As shown in FIG. 2, the jacket structure is provided with an evaporative gas input pipe 36 communicating from the upper part of the cooling medium filling chamber 37 to the lower part of the freezing granulation chamber 31, and liquid nitrogen or When a liquefied gas such as liquid argon is used, the evaporated gas obtained by evaporating the liquefied gas is directly introduced into the lower part of the freezing granulation chamber 31 from the upper part of the cooling medium filling chamber 37 to directly cool the inside of the freezing granulation room 31. It is also possible. Further, in the case of using nitrogen gas, argon gas, dry ice, carbon dioxide gas, or a cooling gas cooled in the atmosphere as a cooling medium, the inside of the freezing granulation chamber 31 is filled by filling the cooling medium filling chamber 37 with these gases. Indirect cooling is also possible, and the inside of the freezing granulation chamber 31 may be directly cooled via the cooling gas supply / exhaust pipe 36 ′ provided in the upper part of the freezing granulation chamber 31.

In the present embodiment, medium remaining amount detecting means 80 for detecting the remaining amount of the cooling medium in the cooling medium filling chamber 37 may be provided. For example, when the cooling medium is a liquid, the medium remaining amount detection means 80 can use various level sensors such as a float type, a displacer type, a guide pulse type, an optical type, an ultrasonic wave, and a laser type. When the medium is a gas body, various concentration sensors such as a semiconductor type, a heat ray type semiconductor type, an infrared type, and an ultrasonic type can be used. Then, by outputting and managing these detection results to an information processing apparatus such as the control computer 81, it is possible to accurately grasp the remaining amount of the cooling medium, the replenishment timing, and the like. Also, the cooling medium remaining amount and the replenishment timing may be notified to the operator via a display unit such as a monitor (not shown) connected via the control computer 81 or a notification unit such as a speaker.

Furthermore, in the present embodiment, cooling medium supplementing means such as a cooling medium supplementing cylinder 82 and a valve 83 may be further provided. In this case, the valve 83 may be opened and closed manually by the operator, or the cooling replenishing means is connected to the control computer 81 via the regulator 84 to detect the remaining amount of the cooling medium and the remaining amount is insufficient. Needless to say, the replenishment in this case is automatically performed via the control computer 81.

The frozen granulation body G formed in the freezing granulation chamber 30 is stored in a freeze-drying unit 50 that is detachably attached to the freezing granulation chamber 30. When a certain amount of the frozen granulation body G is stored in the freeze-drying unit 50, the operator separates the freeze-drying unit 50 from the freeze-granulation chamber 30, and after sealing, freeze-drying to obtain a dry powder. Can do. Below, the structure of the freeze-drying part 50 which concerns on this embodiment is demonstrated.

A detachable storage container that does not have a freeze-drying function is connected to the freeze granulation chamber 30 to store the frozen granulation body G, which is transferred to the freeze-drying unit 50 and dried powder in a later step. You can also get In that case, before transferring the frozen granulated body G, a cooling medium is introduced into the gap 52 through the medium inlet 63 of the casing 52 of the freeze-drying unit 50 described later, and the drying main body 51 is sufficiently cooled. It is preferable to make it. Moreover, there is no problem in cooling by directly putting liquid nitrogen, dry ice or the like into the dry main body 51.

As shown in FIG. 4, the freeze-drying section 50 has a drying main body 51 as a storage container formed in a substantially cylindrical shape with round ends at both ends when the x-axis direction in the figure is the container longitudinal direction; A casing 52 is formed so as to surround the periphery of the drying body 51 and forms a gap 53 with the drying body 51.

A drying portion opening 54 having a substantially circular opening shape is formed in a substantially central portion of the upper body portion of the drying main body 51 so as to protrude through the housing portion 52, and is used for freeze granulation. The frozen granulated body G formed in the chamber 30 is stored in the drying main body 51 through the drying section opening 54. Therefore, as shown in FIG. 5, the drying section opening 54 can be connected and communicated via the granulation chamber side joint 38 formed in the opening 32 at the bottom of the freezing granulation chamber 31. The inner wall portion is formed with a drying portion side joining portion 55 such as a ferrule, a band, a clamp, and a flange. It should be noted that the drying portion side joining portion 55 can be joined to the upper lid 56 for sealing the drying main body portion 51 after the connection with the freezing granulation chamber 30 (freezing granulation chamber 31) is released. It is configured.

Further, a sight glass 57 for observing the inside of the drying main body 51 through the housing 52 is provided on the upper side of the drying main body 51. The operator can observe the storage amount of the frozen granulation G, the progress of freeze-drying, and the like via the sight glass 57. Further, in measuring the storage amount of the frozen granulated body G and the amount of solvent contained therein, a mechanical or optical storage amount detection sensor and an infrared spectroscopic analyzer are provided inside the dry main body 51, and the detection results and analysis results May be output to an information processing apparatus such as the control computer 81.

Similarly, a vacuuming tube connector 59 with a filter is provided on the upper side of the drying main body 51. A cold trap 61 and a vacuum pump 62 are connected to the vacuuming tube connector 59 via a flexible pipe 60. When the vacuum pump 62 is started, the internal pressure (vacuum pressure) inside the drying main body 51 gradually decreases. And the efficiency of lyophilization is achieved by promoting the sublimation of the solvent contained in the frozen granulated body G by circulation of the heat medium to the space | gap part 53 mentioned later and rocking | fluctuation of the freeze-drying part 50 main body. The filter may be attached to the vacuum tube connector, but may be attached between the cold trap 61 and the vacuum pump 62.

After the freeze drying is completed, the operator removes the flexible pipe 60 from the drying main body 50, rotates the drying main body 51 by 180 ° with respect to the container longitudinal axis, and directs the drying section opening 54 toward the floor. A dry powder can be collected by placing a collection container such as a collection tray (not shown) directly below, opening the drying section opening 54 and dropping the dry powder.

The casing 52 has a medium inlet 63 for introducing a heat medium such as heated water, steam, cooling gas, refrigerant oil, and heat transfer oil into a gap 53 formed between the main body 51 and the drying main body 51, and these. A medium discharge port 64 for discharging is provided. Since the gap 53 is formed over substantially the entire area around the drying body 51, the entire drying body 51 can be uniformly heated or cooled. Further, a heat insulating structure equivalent to the heat insulating chamber 34 may be provided on the outer periphery of the gap portion 53.

In addition, the casing 52 has shafts 66 at both ends thereof so that the casing 52 can swing at a predetermined angle with respect to the longitudinal axis 65 when the x-axis direction in the drawing is the longitudinal direction of the container. Is provided. The longitudinal axis 65 and the shaft body 66 may be the center of the drying main body 51, but can be installed on the upper part of the drying main body 51 in order to narrow the movable range of the flexible pipe 60 and reduce consumption. The shaft body 66 is pivotally supported by a bearing 91 provided on the gantry 90, and as shown in FIG. 6, the freeze-drying unit 50 is moved at a predetermined angle (for example, in the longitudinal direction) by a driving force from a motor (not shown). The shaft 65 is configured to be swingable within a movable range of 100 ° left and right in the figure. The freeze-drying part 50 can swing during freeze-drying, that is, the freeze-drying part 50 main body is inclined in the left-right direction with respect to the longitudinal axis of the container. Become. As a result, since the exposure frequency of the surface to be dried of the frozen granulated body G increases and the inside of the bulk body of the frozen granulated body G that is difficult to promote drying is stirred and exposed, the drying efficiency is improved. Can do. In addition, it is possible to prevent the occurrence of drying unevenness that may occur in a stationary freeze dryer. When the flow of the frozen granulated body G is small and stirring is not sufficient, a baffle plate can be set at the bottom inside the dry main body 51 to promote the flow. When the frozen granule G adheres to the dry main body 51 and does not flow, a knocker, a vibrator or the like is installed on the dry main body 51, and the frozen granule G is forced to flow by applying an impact or vibration. You can also.

As described above, in the present embodiment, since the freeze-drying unit 50 is directly connected to the lower part of the freeze-granulation chamber 30, the cold air in the freeze-granulation chamber 31 of the freeze-granulation chamber 30 is lyophilized. It will flow directly into the drying main body 51. As a result, the dried main body 51 is in an appropriately cooled state, thereby eliminating the need for pre-cooling of the collection container, which was necessary in the prior art, and preventing melting of the frozen granule when the container is transferred. be able to.

Next, a method for producing a dry powder by the spray freeze granulated dry powder production apparatus 100 according to the present embodiment having the above-described configuration will be described. In the description here, the case where liquid nitrogen is used as the cooling medium will be described.

First, as an advance preparation, the operator fills the cooling medium filling chamber 37 with liquid nitrogen, and sets the temperature of the freezing granulation chamber 31 to a temperature at which the stock solution M is frozen (approximately −10 ° C. to −190 ° C., preferably −20 ° C. To −150 ° C.). By the way, liquid nitrogen is heat-exchanged and gasified when cooling the freezing granulation chamber 31. By introducing the evaporated nitrogen gas into the freezing granulation chamber 31 via the evaporating gas introduction pipe 36 provided in the cooling medium filling chamber 37, the freezing granulation chamber 31 can be directly cooled more efficiently. It is also possible to put nitrogen gas into the freezing granulation chamber 31 after the spraying of the stock solution M described later is started. Further, nitrogen gas may be directly fed into the inside of the freezing granulation chamber 31 through the cooling gas supply / exhaust pipe 36 ′ provided in the upper part of the freezing granulation chamber 31.

When the room temperature of the freezing granulation chamber 31 is lowered to a temperature at which the stock solution M is frozen, the operator starts spraying the stock solution M from the discharge unit 21 of the two-fluid nozzle main body 11. At this time, by generating a normal temperature or heated gas from the antifreezing gas pipe 20, it is possible to prevent generation and adhesion of frozen solids in the discharge unit 21.

The stock solution M sprayed from the discharge part 21 of the two-fluid nozzle main body part 11 is frozen in the freezing granulation chamber 31 of the freezing granulation chamber 30 to form a freezing granulated body G. The formed frozen granulation body G naturally falls below the freezing granulation chamber 31 and is stored in the drying main body 51 of the freeze drying unit 50 connected to the lower portion of the freezing granulation chamber 31. In addition, when the diameter of the freeze granulation chamber 31 is increased due to an increase in the size of the apparatus intended for mass production or a change in the spraying method, the connection with the freeze drying unit 50 should be a conical hopper. Is also possible. At this time, it is preferable to forcibly drop the frozen granulated body G by applying an impact, vibration, or the like using a knocker, vibrator or the like provided in the hopper. By the way, regardless of whether it is a large machine or a small machine, the liquefied gas is used as an indirect cooling medium, and when the evaporated gas is charged into the freezing granulation chamber 31 via the evaporating gas charging pipe 36 provided in the cooling medium filling chamber 37, Alternatively, when the frozen granulated material G is produced by injecting a large amount of gas by direct cooling instead of indirect cooling using liquefied gas or the like, a cyclone, a bag filter or the like is provided upstream of the cooling gas supply / exhaust pipe 36 '. It is preferable to collect the frozen granulated body G riding on a gas stream.

When the storage amount of the frozen granulation G in the drying main body 51 becomes a certain amount, the operator separates the freeze drying unit 50 from the freezing granulation chamber 30 and joins (attaches) the upper lid 56 to the drying unit opening 54. ) To seal the drying main body 51.

Then, the operator starts evacuation of the inside of the drying main body 51 by starting the vacuum pump 62. Further, the operator starts swinging of the freeze-drying unit 50 by driving a motor (not shown) and rotating the shaft body 66 at a predetermined angle.

In the state where the internal pressure of the drying main body 51 is reduced to a predetermined pressure, for example, a heating medium such as heated water, heating oil, or steam is introduced into the gap 53 through the medium inlet 63 of the housing 52. Thus, the sublimation of the solvent of the frozen granulated body G is promoted. At this time, since the freeze-drying unit 50 main body is inclined in the left-right direction with respect to the longitudinal axis of the container, the frozen granulated body G flows in the drying main body 51 and is further uniformly heated by the conduction electric heat from the heat medium. Will be. Thereby, drying efficiency can be promoted efficiently.

After completion of freeze-drying, the operator places a collection container such as a collection tray (not shown) directly under the drying body 51, removes the flexible pipe 60 from the drying body 51, and removes the drying body 51 in the container longitudinal direction. By rotating 180 ° with respect to the shaft, the drying part opening 54 is directed toward the floor, and the drying part opening 54 is opened to collect the dry powder.

The production of the dry powder according to the present embodiment can be continuously performed by reconnecting the freeze-drying unit 50 after freeze-drying or the separate freeze-drying unit 50 to the freeze granulation chamber 30. At this time, even if the spraying of the stock solution M by the spray mechanism unit 10 is not completely stopped, for example, by continuing spraying in a state where the spray amount is reduced, it is possible to maintain a stable spray state. In addition, instead of reducing the spray amount, a damper is placed directly under the granulation chamber side joint portion 38 so as to be in a closed state, so that the time during which the freeze-drying portion 50 is reconnected is also stable in a sealed state. Can be maintained. Moreover, since the freezing granulation chamber 31 according to the present embodiment can be cooled by indirect cooling using a liquefied gas such as liquid nitrogen as a cooling medium and direct cooling of evaporated nitrogen gas, In this case, it is possible to replenish the cooling medium without affecting the spraying of the stock solution M in the spray mechanism unit 10.

[Modification]
In the preferred example of the spray freeze granulated dry powder production apparatus 100 of the present embodiment, the lyophilization unit 50 that can swing at a predetermined angle with respect to the longitudinal axis of the container has been described as the lyophilization unit. The present invention is not limited to this. For example, as shown in FIG. 7, when the x-axis direction in the figure is the container longitudinal direction, the freezing that can rotate 360 ° with respect to the longitudinal axis 65 ′. The configuration of the drying unit 200 may be used.

The freeze-drying unit 200 is configured to surround a drying main body 51 ′ as a storage container and the periphery of the drying main body 51 ′, and a housing unit that forms a gap 53 ′ between the drying main body 51 ′. 52 ′, the name and function of which can be the same as those of the freeze-drying unit 50. The freeze-drying unit 200 is configured to be able to connect and communicate with the freezing granulation chamber 31 of the freezing granulation chamber 30 through the drying unit opening 54 '.

Also, the freeze-drying section 200 has shaft bodies 66 'formed on the left and right sides of the casing section 52' so that it can be supported by a bearing 91 'provided on the gantry 90'. In order to enable the freeze-drying section 200 to be rotated 360 ° with respect to the longitudinal axis 65 ′, in this modification, the vacuum-evacuation tube connector 59 ′ extends from the central axis of the shaft body 66 ′ to the interior of the drying body 51 ′. Is inserted, and the flexible pipe 60 'is connected to this. By adopting such a connection configuration of the vacuuming tube connector 59 ′, the vacuuming tube connector 59 ′ and the flexible pipe 60 ′ are caught by the gantry 90 ′ or the bearing 91 ′ when the freeze-drying unit 200 is rotated. It is possible to prevent problems such as movement being hindered. Similarly to the freeze-drying unit 50, the freeze-drying unit 200 can rotate during freeze-drying, that is, the freeze-drying unit 200 main body tilts and rotates in the left-right direction with respect to the container longitudinal axis. It will flow in the drying body 51 '. As a result, since the exposure frequency of the surface to be dried of the frozen granulated body G increases, the drying efficiency can be improved.

Furthermore, it is of course possible to configure the freeze-drying unit as a so-called tumbler type rotary drying unit 500 as shown in FIG. The tumbler-type rotary drying unit 500 is configured to surround a drying main body 511 as a storage container and the periphery of the drying main body 511, and a housing 552 that forms a gap 553 with the drying main body 511. Is provided. The tumbler-type rotary drying unit 500 is configured to be able to connect and communicate with the freezing granulation chamber 31 of the freezing granulation chamber 30 through the drying unit opening 554.

The both ends of the tumbler-type rotary drying unit 500 are pivotally supported by the mount 590 so that the tumbler-type rotary drying unit 500 can be rotated 360 ° with respect to the rotation shaft 565. On the left side of the housing portion 552 in the figure, a vacuuming line 559 is inserted into the drying main body portion 511, and on the right side in the drawing, the medium injection line 563 is connected to the gap portion 553.

The drying operation using the tumbler type rotary drying unit 500 can be performed in the same manner as the freeze-drying

units

50 and 200. That is, when the storage amount of the frozen granulation G in the drying main body 511 reaches a certain amount, the operator separates the freeze drying unit 511 from the freezing granulation chamber 30 and joins the upper lid 56 to the drying unit opening 554. By (attaching), the drying main body 511 is sealed.

Then, the operator starts evacuation of the drying main body 511 via the evacuation line 559. Further, the operator starts rotation of the tumbler type rotary drying unit 500 by driving or manually driving a motor (not shown).

In a state where the internal pressure of the drying main body 511 is reduced to a predetermined pressure, for example, by introducing a heat medium such as heated water, heating oil, steam, or the like into the gap 553 through the medium injection line 563, The sublimation of the solvent of the granule G is promoted. At this time, since the tumbler-type rotary drying unit 500 is rotating, the frozen granulated body G flows in the drying main body 511 and is uniformly heated by conduction electric heat from the heat medium. Thereby, drying efficiency can be promoted efficiently.

After the freeze-drying is completed, the operator places a collection container such as a collection tray (not shown) immediately below the drying main body 511, rotates the drying main body 511 by 180 ° with respect to the rotation axis, and opens the drying unit. The part 554 is directed toward the floor, the drying part opening 554 is opened, and the dry powder is collected.

In addition, in this invention, the structure as a freeze-drying part is not limited to the said example. That is, as shown in FIG. 9, a storage container having a so-called stationary shallow shape provided with a drying portion opening 354 that can be connected to and communicated with the freezing granulation chamber 31 of the freezing granulation chamber 30. May be used as the freeze-drying unit 300. Considering the efficiency of lyophilization, the storage amount is limited, but as in the above example, the cold air in the freezing granulation chamber 31 of the freezing granulation chamber 30 flows directly into the drying main body of the freezing drying unit 300. Therefore, there is no need for the prior cooling of the collection container, which is necessary in the prior art, and it is possible to prevent the frozen granulation from being melted when the container is transferred. In order to increase the exposure frequency of the surface to be dried of the frozen granulated body G, for example, as shown in FIG. 10, a stirring member such as a stirring blade that stirs the frozen granulated body G stored in the drying main body. Of course, it is possible to use the storage container provided with 301 as the freeze-drying unit 300 ′.

In the preferred description of the present invention, an example in which one lyophilization unit is used has been described. However, for example, it is of course possible to operate a plurality of lyophilization units simultaneously. Specifically, a pipe for transportation that extends from the lower part of the chamber for freezing granulation and is provided with stirring and transporting means such as a helical blade is provided, and a plurality of frozen granulation bodies transported by the transportation pipe are provided. It is possible to obtain a form close to full automation by sequentially receiving it in the freeze-drying section and starting freeze-drying in order from the amount in which the storage amount exceeds a certain amount. In this case, it is necessary to cool a plurality of freeze-drying units in advance, but the gas, oil, ethylene glycol-containing liquid, propylene glycol cooled through the medium inlet provided in the casing of the freeze-drying unit By introducing an antifreeze liquid such as a containing liquid in advance, the dry main body can be appropriately cooled. An operator can obtain a dry powder by connecting a vacuum line to a freeze-drying section ready for freeze-drying and starting freeze-drying, and thus can further improve productivity.

By the way, when the cooling medium sent to the freezing granulation chamber is exhausted, the collecting means for collecting the freezing granulated material discharged on the airflow is produced by the spray freezing granulated dry powder production according to this embodiment. By providing the apparatus, it is also possible to construct a spray freeze granulated powder production system aiming at further yield improvement.

FIG. 11 is a system configuration diagram illustrating an example of a configuration example of the spray freeze granulated dry powder manufacturing system 700. In this description, the spray freeze granulated dry powder production apparatus is intended for mass production of frozen granulated bodies, and is connected to the freeze dry section via a conical hopper section. A spray freeze granulated dry powder production apparatus 600 including the centrifugal sprayer 400 illustrated in FIG. 3 as an example of a spray mechanism provided in the mechanism unit will be described as an example.

The air drawn in by the blower 618 through the gas suction filter 617 is passed through the heat exchanger 615 cooled by the chiller 619 to become cooled atmospheric gas. The cooling atmospheric gas is introduced into the freezing granulation chamber 631 in the freezing granulation chamber 630 through the cooling gas supply pipe 624 through the filter 623. At this time, since moisture contained in the atmosphere adheres as frost to the heat exchanger 615, there is a risk of hindering long-time operation. Therefore, it is preferable to attach a dehumidifier 621 to the front stage of the heat exchanger 615. . As the cooling gas, the cooling air gas described here may be used, and it is of course possible to use a cooling gas such as nitrogen gas, argon gas, helium gas, carbon dioxide gas or the like. The freezing granulation chamber 630 may be cooled by indirect cooling using the jacket structure described above. In this case, when the jacket structure is provided with an evaporative gas input pipe and a liquefied gas such as liquid nitrogen or liquid argon is used as a cooling medium, the evaporated gas evaporated from the liquefied gas is directly frozen from the upper part of the jacket structure. It is preferable to adopt a configuration in which the particle chamber 631 is directly introduced into the lower portion.

The stock solution M in the stock solution tank 613 is supplied to the centrifugal sprayer 400 via the stock solution supply pipe 612 by the pump 614. Centrifugal sprayer 400 atomizes supplied stock solution M by centrifugal spraying. The undiluted undiluted solution M is solidified by contact with the cooled atmospheric gas supplied through the cooling gas supply pipe 624 to form a frozen granulated body G. In the vicinity of the rotating disk unit 402 of the centrifugal sprayer 400, a cooling gas heat shield plate 634 having a shape surrounding the rotating disk unit 402 is provided. A gas suction filter 617 ′, a blower blower 618 ′, and a heater 622 are provided in front of the cooling gas heat shield plate 634. The blower 618 'draws in gas such as the atmosphere through the gas suction filter 617'. The gas heated at room temperature or by the heater 622 is input to the inside of the cooling gas heat shield plate 634 through the antifreeze gas pipe 620, and generation and adhesion of frozen solids to the rotating disk 402 can be suppressed. Similarly to the cooling gas supply line described above, the dehumidifier 621 ′ is provided between the blower blower 618 ′ and the heater 622 ′, thereby reducing the water introduced into the freezing granulation chamber 631 and freezing. It is also possible to suppress the generation of frost in the grain chamber 631.

The frozen granulation G generated in the freezing granulation chamber 631 is deposited on the conical hopper 632 located below the freezing granulation chamber 631 in the freezing granulation chamber 630 and provided in the hopper 632. It is forcibly dropped to the above-mentioned freeze-drying part by the impact and vibration by a knocker 633, a vibrator or the like. When the storage amount of the granulation body G in the freeze-drying unit becomes a certain amount, the operator can separate the freeze-drying unit from the freeze-granulating chamber 630, and after sealing, freeze-drying can obtain a dry powder. .

Note that a cooling gas exhaust pipe 625 for exhausting the cooling atmospheric gas introduced into the freezing granulation chamber 631 is connected to the hopper portion 632. The cooling gas exhaust pipe 625 is provided with a cyclone type dust collector 626 as a collecting means for collecting the fine frozen granule G discharged on the airflow when the cooling atmospheric gas is exhausted. Is provided. The frozen granulated material G collected by the cyclone type dust collector 626 can be collected by a freeze-drying unit provided at the lower part of the cyclone type dust collector 626. Further, a bag filter type dust collector 628 as a collecting means for collecting a finer frozen granulated material G that cannot be collected by the cyclone type dust collector 626 is provided at the upper end of the cyclone type dust collector 626. Are connected via a cooling gas exhaust pipe 627. The frozen granulated material G collected by the bag filter type dust collector 628 can be collected by a freeze-drying unit provided at the lower part of the bag filter type dust collector 628. In addition, the aggregated piping of the frozen granulation G is installed in the lower part of the hopper part 632, the cyclone type dust collector 626, and the bag filter type dust collector 628, or a plurality of frozen granule G inlets are provided in the freeze drying part. By providing, it can also collect in one freeze-drying part. The cyclone type dust collector 626 and the bag filter type dust collector 628 are provided with a knocker 633, a vibrator and the like as with the hopper portion 632, and the frozen granule G is forced to the freeze drying portion by the impact and vibration caused by them. It may be dropped. In the description here, the configuration in which the cooling gas exhaust pipe 625 is provided in the hopper portion 632 has been described, but the cooling gas exhaust pipe 625 may be provided in the freezing granulation chamber 631 side.

Although the cooled atmospheric gas that has passed through the bag filter type dust collector 628 can be discharged into the atmosphere by the exhaust blower 629, a circulation pipe 640 indicated by a dotted line in the figure is connected to circulate before the blower blower 618. By doing so, the cooling atmospheric gas can be reused.

Thus, when the cooling medium sent to the freezing granulation chamber is exhausted, the collection / recovery means for collecting and recovering the frozen granulated material discharged on the air current is spray-freezing according to this embodiment. By providing it to the granulated dry powder production apparatus, it is also possible to provide a spray-frozen granulated powder production system aiming at further yield improvement.

As described above, according to the present invention, the spray freeze-granulated dry powder production apparatus and spray freeze-granulated powder are capable of mass production of dry powder by continuous operation and long-time operation, eliminating manual steps as much as possible. A manufacturing system can be provided.

DESCRIPTION OF SYMBOLS 10 Spray mechanism part 11 Two-fluid nozzle main-body part 12,612 Stock solution supply pipe | tube 13,613 Stock solution tank 14,614 Pump 15 Compressed gas supply pipe | tube 16 Compressed gas supply part 17,617,617 'Gas suction filter 18,618,618' Blower blower 19 HEPA filter 20, 620 Antifreeze gas piping 21 Discharge part 22, 622 Heater 30, 630 Freezing granulation chamber 31, 631 Freezing granulation room 32 Opening 33 Freezing granulation room outer wall 34 Insulating room 35 Insulating room wall 36 Evaporative gas introduction pipe 36 ′ Cooling gas supply / exhaust pipe 37 Cooling medium filling chamber 38 Granulation chamber side joint portion 39 Heat insulation chamber outer wall 40 Support members 50, 200, 300, 300 ′, 500 Freeze drying portions 51, 51 ′, 511 Drying main body 52, 52 ′, 552 Housing 53, 53 ′, 553 Gap 54, 54 ′, 354, 554 Drying Mouth part 55 Drying part side joint part 56 Upper cover 57 Sight glass 59 Vacuum pulling tube connector 60 Flexible piping 61 Cold trap 62 Vacuum pump 63 Medium inlet 64 Medium outlet 65, 65 'Longitudinal central axis 66, 66' Shaft 70 Stand 80 Medium remaining amount detection means 81 Control computer 82 Refill cylinder 83 Valve 84 Regulator 90, 90 ', 590 Mount 91, 91' Bearing 100, 600 Spray freeze granulated dry powder production apparatus 301 Stirring member 400 Centrifugal sprayer 401 Motor part 402 Rotating disk part 559 Vacuum drawing line 563 Medium injection line 565 Rotating shaft 615 Heat exchanger 619 Chiller 621, 621 'Dehumidifier 623 Filter 624 Cooling gas supply pipe 625, 627 Cooling gas exhaust pipe 626 Cyclone type dust collecting Device 628 Bug filter type collection Device 629 exhaust air blower 632 hopper 633 knocker 634 circulation pipe cooling gas heat shield 640 700 spray freeze granulated dry powder production systems

Claims

Spray freeze granulation drying in which a frozen granulation is produced in a freezing granulation chamber by cooling a continuously supplied stock solution, and the produced frozen granulation is freeze dried to produce a dry powder. A powder manufacturing apparatus,
A spray mechanism having spray preventing means and spraying the stock solution into the freeze granulation chamber;
The freezing granulation chamber has a storage container configured to be detachable in the lower part of the freezing granulation chamber and storing the freezing granulation body generated in the freezing granulation chamber, and the freezing granulation body stored in the storage container A freeze-drying section for freeze-drying,
The freezing granulation chamber directly cools by introducing a cooling medium directly into the chamber and cooling, and indirectly by cooling the jacket structure provided around the freezing granulation chamber with the cooling medium. A spray freeze granulated dry powder production apparatus characterized by being cooled by any one of cooling or a combination thereof.
2. The spray freeze granulated dry powder production according to claim 1, wherein the jacket structure is provided with an evaporative gas input pipe for directly introducing evaporative gas obtained by evaporating the filled cooling medium into the chamber. apparatus.
The spray-freeze-granulated dry powder production apparatus according to claim 1, wherein the storage container is formed so as to be swingable at a predetermined angle with respect to the longitudinal axis of the container.
The spray-freeze-granulated dry powder manufacturing apparatus according to claim 1, wherein the storage container is formed so as to be rotatable with respect to the longitudinal axis of the container.
The spray frozen granulated dry powder production apparatus according to claim 1, wherein the storage container is formed in a shallow bottom shape in which the frozen granulated body is allowed to stand.
The spray frozen granulated dry powder production apparatus according to claim 1, wherein the storage container includes a stirring member that stirs the stored frozen granulated body.
2. The spray freeze granulated dry powder production according to claim 1, wherein the spray mechanism includes a spray mechanism of any one of a two-fluid nozzle, a one-fluid pressurizing nozzle, an ultrasonic nozzle, and a centrifugal sprayer. apparatus.
The spray freeze granulated dry powder according to claim 7, wherein the freeze prevention means includes an antifreeze gas supply unit that supplies an antifreeze gas at normal temperature or warm temperature in the vicinity of the stock solution discharge unit of the spray mechanism. Body manufacturing equipment.
The cooling medium is any one of liquid nitrogen, nitrogen gas, liquid argon, argon gas, liquid helium, helium gas, dry ice, carbon dioxide gas, or a cooling gas that cools the atmosphere. The spray freeze granulated dry powder production apparatus described in 1.
The spray frozen granulated dry powder manufacturing apparatus according to claim 1, further comprising medium remaining amount detecting means for detecting the remaining amount of the cooling medium in the jacket structure.
The spray freeze granulated dry powder manufacturing apparatus according to claim 10, further comprising a cooling medium replenishing unit that replenishes the cooling medium in the jacket structure based on a detection result by the medium remaining amount detecting unit.
The spray frozen granulated dry powder production apparatus according to claim 1, wherein the jacket structure includes a heat insulating structure.
Spray freezing in which a frozen granulation body is produced from a continuously supplied stock solution in a freezing granulation chamber into which a cooling medium has been introduced, and the produced frozen granulation body is freeze-dried to produce a dry powder. A dry powder manufacturing system,
A spray mechanism having spray preventing means and spraying the stock solution into the freeze granulation chamber;
The freezing granulation chamber has a storage container configured to be detachable in the lower part of the freezing granulation chamber and storing the freezing granulation body generated in the freezing granulation chamber, and the freezing granulation body stored in the storage container A freeze-drying section for freeze-drying;
A spray freeze-dried powder production system, comprising: a collecting unit that collects the frozen granule that moves as the cooling medium is exhausted.
The spray freeze-dried powder manufacturing system according to claim 13, wherein the collecting means includes a cyclone type dust collector and / or a bag filter type dust collector.