Particle manufacturing apparatus and method for manufacturing frozen particles

Abstract

The present invention provides a particle manufacturing apparatus capable of rapidly manufacturing frozen particles while minimizing nozzle clogging due to freezing, and a method for manufacturing frozen particles. The present invention provides a particle manufacturing apparatus, comprising: a freezing chamber for accommodating frozen particles in which an object to be treated containing moisture is frozen in the form of particles; the present invention relates to a freezing apparatus comprising a freezing chamber, an ultrasonic nozzle that converts an object to be treated into a particulate form after or before freezing and discharges the resulting object into the freezing chamber, and a pressure reducing device for reducing the pressure of the freezing chamber, in which moisture in the frozen particulate is evaporated as a result of the pressure reduction, and the frozen particles are cooled and frozen due to evaporation of moisture.

Description

[0001] CROSS-REFERENCE TO RELATED APPLICATIONS

[0002] This application claims the benefit of Japanese Patent Application No. 2022-82477 and Japanese Patent Application No. 2023-3947, the contents of which are hereby incorporated by reference herein. Technical Field

[0003] The present invention relates to a particle manufacturing device and a particle manufacturing method, and more particularly, to a particle manufacturing device for manufacturing frozen particles and a method for manufacturing frozen particles. Background Art

[0004] In the related art, freeze-dried food is referred to as long-term storage food, etc. Freeze-dried food is prepared by freezing cooked rice, vegetables, etc., and removing moisture under reduced pressure. In addition, liquids such as juices are also freeze-dried (for example, Patent Document 1 below). In addition, not only food and beverages, but also various other things are used as objects to be freeze-dried (objects to be processed).

[0005] Patent document 1 below describes that a freeze-dried part contains frozen particles and is evacuated in a sealed state to prepare freeze-dried particles. The patent document describes a method for containing frozen particles in a freeze-dried part, wherein the freeze-dried part is open upward, a vertical cylindrical freezing granulation chamber maintained at a low temperature is arranged in the upper part of the freeze-dried part, liquid is sprayed from the upper end of the freezing granulation chamber through a nozzle, the sprayed liquid particles are frozen in the freezing granulation chamber, and the frozen particles fall into the freeze-dried part.

[0006] Citation List

[0007] Patent Literature

[0008] Patent Document 1: WO 2019 / 175954 Summary of the invention

[0009] Technical issues

[0010] In the prior art method, it takes time for liquid particles discharged from the nozzle to become frozen, so the freezing granulation chamber needs to have a certain height, which makes the equipment large-scale. It is conceivable to lower the temperature of the freezing granulation chamber, but this may cause the nozzle to freeze and clog. Therefore, a particle manufacturing device for manufacturing frozen particles is needed to quickly freeze the particles discharged from the nozzle, but this requirement has not been met. Therefore, the object of the present invention is to provide a particle manufacturing device and a method for manufacturing frozen particles that can quickly manufacture frozen particles while preventing nozzle clogging due to freezing.

[0011] Solution to the problem

[0012] The present invention for solving the above-mentioned problems provides a particle manufacturing device, comprising:

[0013] a freezing chamber configured to accommodate frozen particles obtained by freezing an object to be processed in the form of particles containing moisture;

[0014] a decompression device configured to decompress the freezing chamber, and

[0015] an ultrasonic nozzle configured to discharge the object to be processed in the form of particles into the freezing chamber depressurized by the depressurizing device, wherein

[0016] The frozen particles are produced as a result of freezing the object to be processed by evaporation of moisture from the object to be processed under a reduced pressure environment.

[0017] In order to solve the above problems, the present invention provides a method for producing frozen particles, comprising:

[0018] forming the object to be processed containing moisture into a granular form by an ultrasonic nozzle; and

[0019] before the object to be processed is formed into a particle form by the ultrasonic nozzle, or after the object to be processed is formed into a particle form by the ultrasonic nozzle, freezing the object to be processed to produce frozen particles, wherein the object to be processed is frozen in the particle form,

[0020] The freezing of the object to be processed is achieved by cooling the object to be processed, and the cooling is caused by evaporation of water. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] [ Figure 1 ] Figure 1 : is a schematic diagram showing the structure of the particle production apparatus according to the first embodiment.

[0022] [ Figure 2A ] Figure 2A is a schematic diagram showing the structure of an ultrasonic nozzle.

[0023] [ Figure 2B ] Figure 2B It is a schematic diagram showing a usage state of the ultrasonic nozzle.

[0024] [ Figure 2C ] Figure 2C is a schematic diagram showing the structure of another ultrasonic nozzle.

[0025] [ Figure 2D ] Figure 2Dis a schematic diagram showing the structure of another ultrasonic nozzle.

[0026] [ Figure 3A ] Figure 3A : is a schematic diagram showing the structure of a particle production apparatus according to a second embodiment.

[0027] [ Figure 3B ] Figure 3B is a schematic plan view showing the arrangement of ultrasonic nozzles in the particle manufacturing apparatus of the second embodiment (along the Figure 3A (a view taken in the direction of arrow B in FIG. 1 ).

[0028] [ Figure 3C ] Figure 3C is shown with Figure 3B Arrangements of ultrasonic nozzles Schematic plan views of different arrangements of ultrasonic nozzles.

[0029] [ Figure 3D ] Figure 3D is shown with Figure 3C A schematic plan view of a state in which an object to be processed is discharged from an ultrasonic nozzle in different directions.

[0030] [ Figure 3E ] Figure 3E is a schematic perspective view showing a preferred arrangement of ultrasonic nozzles.

[0031] [ Figure 4A ] Figure 4A is a schematic front view showing a state in which an object to be processed is discharged from an ultrasonic nozzle.

[0032] [ Figure 4B ] Figure 4B : is a schematic front view showing a state where an object to be processed is discharged from an ultrasonic nozzle.

[0033] [ Figure 5 ] Figure 5 : is a schematic diagram showing the structure of a particle production apparatus according to a third embodiment.

[0034] [ Figure 6 ] Figure 6 : is a schematic diagram showing the structure of a particle production apparatus according to a fourth embodiment. DETAILED DESCRIPTION

[0035] Hereinafter, embodiments of the present invention will be described with reference to the accompanying drawings. In the particle manufacturing device of the prior art, frozen particles are formed by discharging liquid in the form of particles into a cooling space. In the present embodiment, an object to be processed containing moisture is supplied to a reduced pressure environment. At this time, the moisture is evaporated to freeze the object to be processed. That is, in the present embodiment, evaporation heat is used to freeze the object to be processed. Compared with the method in the prior art, freezing the object to be processed by evaporation heat can be performed faster. An ultrasonic nozzle is used to discharge the object to be processed, so in the present embodiment, clogging caused by freezing of the object to be processed at the nozzle can be prevented.

[0036] First, a particle manufacturing device will be described. The particle manufacturing device according to the present embodiment is a device for manufacturing frozen particles formed by freezing a liquid object to be processed. The frozen particles in the present embodiment can be restored to room temperature and constant pressure (for example, 23°C and 1 constant pressure (atm)), and restored to a liquid state in a state where the frozen state is released. The particle manufacturing device of the present invention is used not only to form frozen particles that are restored to a liquid state at room temperature, but also to form freeze-dried particles that can maintain a solid state by drying such frozen particles even in a state where the frozen state is released.

[0037] The liquid object to be processed may be an object containing only liquid or a slurry containing liquid and solid particles. In the present embodiment, a liquid material is described as an example of the object to be processed, but the object to be processed as frozen particles is not limited to a liquid material, and may be a solid or semi-solid material (such as a jelly or paste material) as long as it can be granulated by ultrasonic vibration.

[0038] (First embodiment)

[0039] Figure 1 The particle manufacturing device 100 according to the first embodiment is illustrated, and the particle manufacturing device 100 according to the first embodiment includes a freezing chamber 10 in which a liquid object to be processed (hereinafter, also referred to as "raw liquid L") is frozen, a decompression device 20 that decompresses the freezing chamber 10, and a discharge device 30 that discharges the raw liquid in the form of particles into the freezing chamber 10. In the freezing chamber 10 of the present embodiment, frozen particles A having a lower moisture content than the object to be processed (raw liquid L) are formed. For example, the discharge device 30 of the present embodiment may be configured to discharge the raw liquid into the freezing chamber 10 without freezing the raw liquid. The discharge device 30 of the present embodiment may be configured to discharge the raw liquid into the freezing chamber 10 after freezing the raw liquid. That is, the discharge device 30 of the present embodiment may be configured to freeze at least a portion of the raw liquid into particles and then discharge them into the freezing chamber 10.

[0040] In the freezing chamber 10, the discharged raw liquid L has a fine particle form, water W evaporates from each particle, and frozen particles A having a water content W smaller than that of the raw liquid L are produced by evaporation heat due to the evaporation of the water content W. In the present embodiment, the frozen particles obtained by freezing the raw liquid L are discharged from the discharge device 30 to the freezing chamber 10, and the water content W is further evaporated from the frozen particles A in the freezing chamber 10. That is, the freezing chamber 10 of the present embodiment is configured to accommodate frozen particles obtained by freezing the raw liquid L into a particle form.

[0041] The freezing chamber 10 has a housing space 10a for housing frozen particles A. The particle production apparatus 100 is configured not only to keep the housing space 10a in a sealed state but also to adjust the housing space 10a to a predetermined reduced pressure state (vacuum degree) by exhausting the housing space 10a with the decompression device 20 .

[0042] The freezing chamber 10 can adjust the temperature of the wall surface in contact with the frozen particles A. For example, the freezing chamber 10 can adjust the temperature of the wall surface to a low temperature so that the frozen particles A can be easily kept in a frozen state. The temperature of the wall surface can be adjusted by attaching a Peltier element or the like. For example, the temperature of the wall surface can be adjusted by using the following method, that is, passing a heat medium through a jacket portion formed by making the wall into a double-layer structure.

[0043] The decompression device 20 of the present embodiment includes a vacuum pump 21 for performing evacuation. The vacuum pump 21 may be a general type such as a reciprocating pump, a rotary pump, and a diffusion pump.

[0044] The discharge device 30 of this embodiment includes an ultrasonic nozzle 31 for discharging the object to be processed into the accommodation space 10a of the freezing chamber 10 and a pump 32 for sending the raw material liquid L to the ultrasonic nozzle 31. Figure 2A As shown, the ultrasonic nozzle 31 has a discharge port 31a for discharging the object to be processed. The pump 32 may be a common pump, such as a reciprocating pump (such as a piston pump, a diaphragm pump and a plunger pump) or a positive displacement pump (such as a gear pump, a vane pump and a screw pump).

[0045] The discharge device 30 can discharge the object to be processed so that the object to be processed is discharged forcibly or slowly. The discharge device 30 can discharge the object to be processed in the form of fine mist or in the form of large particles.

[0046] In the nozzle of the prior art, in which the liquid is formed into a particle form by discharging the liquid through a narrow flow channel at a high speed, freezing is likely to occur in the flow channel. On the other hand, the ultrasonic nozzle 31 can discharge the object to be processed in the form of fine particles by applying ultrasonic vibrations, so it is not always necessary to provide such a narrow flow channel, and when such a narrow flow channel is provided, the nozzle can also be prevented from being blocked because the frozen object in the flow channel is easily decomposed by the ultrasonic vibration. Therefore, in the present embodiment using the ultrasonic nozzle, even if the object to be processed is not in a liquid state but a solid object, the object to be processed can also be discharged into the accommodation space in the form of particles. Therefore, as will be described in detail later, in the ultrasonic nozzle 31 of the present embodiment, the frozen particles A can be formed with the ultrasonic nozzle 31 and then discharged toward the freezing chamber 10. That is, the ultrasonic nozzle 31 of the present embodiment can freeze the object to be processed inside or on its surface.

[0047] The ultrasonic nozzle 31 according to the present embodiment may be configured to discharge the object to be processed in the form of fine particles by applying ultrasonic vibration to the object to be processed before or after freezing. Figure 2A Ultrasonic nozzle shown.

[0048] Figure 2A The ultrasonic nozzle 31 shown includes a cylindrical nozzle body 311, a housing 312, and an ultrasonic vibrator 313, the distal end portion of the cylindrical nozzle body 311 is opened as a discharge port 31a, the housing 312 covers the nozzle body 311, and the ultrasonic vibrator 313 is used to vibrate the nozzle body 311. For example, the ultrasonic vibrator 313 of this embodiment can be an electrostrictive element or a magnetostrictive element. In the ultrasonic nozzle 31 of this embodiment, the vibration frequency of the ultrasonic vibrator 313 can be adjusted. For example, the frequency of the ultrasonic vibrator 313 can be changed between 20kHz and 130kHz.

[0049] The nozzle body 311 includes a cylindrical portion 3110 constituting a flow passage 311b of the raw material liquid L. In the nozzle body 311, one end of the flow passage 311b is opened as a discharge port 31a. The nozzle body 311 also includes a flange portion 3111 extending outward from an end edge portion of the cylindrical portion 3110 defining the discharge port 31a. The raw material liquid L reaching the discharge port 31a through the flow passage 311b is changed into a fine particle form due to the vibration of the distal end portion of the nozzle body 311 and is discharged from the discharge port 31a.

[0050] The nozzle body 311 includes a flange portion 3111 having a surface extending outwardly from the discharge port 31a in a radial direction. The nozzle body 311 has the discharge port 31a at a position corresponding to the center of the flange portion 3111. The nozzle body 311 is configured to discharge the raw material liquid L after temporarily holding the raw material liquid L on the surface 3111a of the flange portion 3111, rather than directly discharging the raw material liquid L from the discharge port 31a into the accommodation space 10a.

[0051] The nozzle body 311 of the present embodiment extends from the housing 312 in a rod shape, and the base end side of the nozzle body is a fixed end fixed to the housing 312, and the open distal end portion of the discharge port 31a is a free end, so the vibration direction of the distal end portion is the plane direction of the flange portion 3111. Therefore, the raw material liquid L flowing out from the discharge port 31a temporarily moves laterally along the surface of the flange portion 3111. Then, the raw material liquid L is temporarily held on the surface of the flange portion 3111, and then discharged into the accommodation space 10a in the form of particles. That is, the flange portion 3111 of the ultrasonic nozzle 31 of the present embodiment is a holding portion that holds the object to be processed (raw material liquid L). In the present embodiment, the holding portion (flange portion 3111) has a surface 311a exposed in the accommodation space 10a. The holding portion (flange portion 3111) in the present embodiment is configured so that the object to be processed (raw material liquid L) discharged from the discharge port 31a can be temporarily held at the surface 311a.

[0052] In this embodiment, the ultrasonic nozzle 31 has the above-mentioned structure, so Figure 2B As shown, a part or all of the raw material liquid L can be frozen on the surface 3111a of the flange portion 3111. That is, in the present embodiment, at least a part of the frozen particles A can be formed in the ultrasonic nozzle 31. In order to freeze the raw material liquid L before discharging the raw material liquid L from the ultrasonic nozzle 31, the temperature of the raw material liquid L supplied to the ultrasonic nozzle 31 can be lowered. In addition, by further lowering the air pressure in the accommodating space 10a, the raw material liquid L can be frozen before discharging the raw material liquid L from the ultrasonic nozzle 31. As described above, the ultrasonic nozzle of the present embodiment is configured to freeze the object to be processed (raw material liquid L) on the surface 311a of the holding portion (flange portion 3111) to form the frozen particles A, and discharge the formed frozen particles A from the surface 311a.

[0053] Because the raw material liquid L is temporarily held on the surface of the flange portion 3111, the temperature of the raw material liquid L is reduced before the raw material liquid L is discharged, but the holding time in the flange portion 31111 is affected by surface tension and the like. The ultrasonic nozzle 31 can discharge the raw material liquid L in the form of small particles. As described above, in the present embodiment, the particles discharged from the ultrasonic nozzle 31 may be only particles before being frozen, or may include particles before being frozen and frozen particles A. In the present embodiment, the particles discharged from the ultrasonic nozzle 31 may be only frozen particles A. The frozen particles A have less moisture content and are lighter than the particles before being frozen. In addition, the particles before being frozen are also reduced in weight by being refined. Therefore, the particles of the discharged raw material liquid L fall slowly. In the present embodiment, since the particles of the raw material liquid L whose temperature is reduced by being held in the flange portion 3111 can fall slowly, the falling distance required for the discharged particles to become frozen particles having a desired temperature is shortened, and the device size can be made compact. The advantages obtained by using the ultrasonic nozzle 31 and the advantages obtained by setting a holding portion in the ultrasonic nozzle 31 to freeze and then discharge the object to be processed also apply to the particle manufacturing device 101 of the second embodiment, the particle manufacturing device 102 of the third embodiment and the particle manufacturing device 103 of the fourth embodiment to be described later.

[0054] In the present embodiment, the vibration frequency of the ultrasonic vibrator 313 can be adjusted, so that the particle size of the raw liquid L to be discharged from the discharge port 31a can be changed. That is, in the present embodiment, by increasing the vibration frequency of the ultrasonic vibrator 313 (shortening the wavelength), the size of the particles can be made finer and smaller, and particles having a large specific surface area from which water may be evaporated can be formed. The particles of the raw liquid L having a large specific surface area are discharged into the accommodation space 10a of the freezing chamber 10 under a reduced pressure state, and become frozen particles A when water W evaporates from the surface of the particles, and the temperature of the particles decreases due to the evaporation heat of water W.

[0055] The particle manufacturing device 100 of the present embodiment can form frozen particles A before being discharged from the ultrasonic nozzle 31. In addition, when the particles before being frozen are discharged from the ultrasonic nozzle 31, the particle manufacturing device 100 of the present embodiment can also quickly freeze the particles after discharge. The adhesion of the frozen particles A is lower than that of the particles before being frozen. Therefore, in the present embodiment, it is possible to prevent the frozen particles A from adhering to the wall surface of the freezing chamber 10 that defines the accommodating space 10a, etc., or reduce the formation of agglomerates that aggregate multiple frozen particles A. These advantages also apply to the particle manufacturing device 101 of the second embodiment, the particle manufacturing device 102 of the third embodiment, and the particle manufacturing device 103 of the fourth embodiment, which will be described later.

[0056] In a general spraying device, the liquid is forcibly discharged from a small nozzle hole, so that the liquid becomes a fine mist. Therefore, in a general spraying device, the channel resistance of the liquid in the nozzle is large, and a pressure of 0.1 MPa or more is applied to the liquid. On the other hand, in the present embodiment, the nozzle body 311 having the discharge port 31a vibrates to turn the raw material liquid L to be discharged from the discharge port 31a into fine particles. In the present embodiment, the raw material liquid L is refined by the kinetic energy generated by the vibration of the nozzle body 311, and the pressure of the raw material liquid L before being supplied to the ultrasonic nozzle 31 can be set to 50 kPa or less, which can greatly reduce the load of the pump 32.

[0057] In the present embodiment, the discharge port 31a is opened in the decompressed accommodation space 10a, and the raw material liquid L is sucked from the accommodation space 10a side, so the supply pressure of the raw material liquid L to the ultrasonic nozzle 31 can be further reduced. The pressure may be 40 kPa or less, or may be 30 kPa or less. For example, the pressure is 1 kPa or more.

[0058] The discharge port 31a of the ultrasonic nozzle 31 is open to the freezing chamber 10 in the decompressed state. Therefore, the space constituting the flow channel 311b inside the nozzle body 311 is communicated with the accommodating space 10a via the discharge port 31a. In other words, the space inside the ultrasonic nozzle 31 is decompressed by the decompression device 20 together with the freezing chamber 10. Therefore, when the open area of ​​the discharge port 31a (the cross-sectional area of ​​the flow channel 311b) increases, negative pressure is easily applied to the flow channel 311b upstream of the discharge port 31a. In this case, when a situation occurs in which the supply of the raw material liquid L is restricted and it is unlikely that the raw material liquid L is discharged from the discharge port 31a, water may evaporate from the raw material liquid L at a position deeper than the discharge port 31a. When the cross-sectional area of ​​the flow channel 311b is large, water vapor generated by the evaporation of water may be discharged into the freezing chamber 10 through the discharge port 31a. Therefore, the flow channel 311b is closed by the frozen object generated by the freezing of the raw material liquid L at a position deeper than the discharge port 31a.

[0059] In the present embodiment, even when the raw liquid L is frozen to block the flow channel 311a in the middle of the flow channel 311b, the frozen object can be crushed due to the vibration of the nozzle body 311, and the frozen particles A obtained by crushing the frozen object can be discharged from the discharge port 31a. In addition, even if the frozen object blocking the flow channel 311b is not crushed, friction heat can be generated due to the vibration at the interface between the wall surface of the flow channel 311b and the frozen object, and the surface layer portion of the frozen object can be liquefied, so the frozen object can be moved toward the discharge port 31a by using the suction force from the accommodating space 10a side, and the frozen object can be granulated to form the frozen particles A when being discharged from the discharge port 31a.

[0060] The pressure in the accommodating space 10a is generally determined based on the balance between the amount of water evaporated from the discharged raw material liquid L and the exhaust volume of the vacuum pump 21. In the ultrasonic nozzle 31 of the present embodiment, the necessity of applying pressure to the raw material liquid L is low, so as required, the cross-sectional area of ​​the flow channel 311b immediately before the discharge port 31a can be made larger than that of a general nozzle, and the occurrence of temporal variation in the discharge volume of the raw material liquid L can be prevented.

[0061] For example, when the raw liquid L is a material containing dietary fiber (such as fruit juice) or a slurry containing fine particles, when the flow channel is narrow, the dietary fiber or fine particles may remain in the flow channel and may become an obstacle to the flow of the liquid. When such an obstacle appears, the amount of liquid discharged will be reduced. In addition, when the obstacle is accidentally removed, the amount of liquid discharged can be restored. This may produce a large fluctuation range of the amount of liquid discharged. When the amount of liquid discharged into the decompression space fluctuates, the pressure balance of the space may be lost, resulting in large pressure fluctuations. On the other hand, in the present embodiment, such a problem can be prevented from occurring.

[0062] When the amount of discharged liquid fluctuates, the size of the liquid particles also changes, and when a large amount of liquid is discharged, the vacuum degree decreases (the absolute pressure increases), which may cause insufficient freezing of the liquid, and the frozen particles that have been formed may coalesce with the insufficiently frozen liquid. In the present embodiment, the amount of the raw material liquid L to be discharged into the accommodating space 10a is less likely to fluctuate, so such a problem is less likely to occur, and frozen particles having a uniform size can be prepared.

[0063] In the ultrasonic nozzle 31 of the present embodiment, clogging due to freezing can be prevented from being easily ensured from the perspective of ensuring a large cross-sectional area of ​​the flow passage 31b immediately before the discharge port 31a. However, it is possible that clogging due to freezing may occur due to unexpected factors, so it is desirable to provide a mechanism that can quickly eliminate clogging and restore the discharge of the raw liquid L, in preparation for the occurrence of clogging.

[0064] The housing 312 in this embodiment has a cylindrical shape whose inner diameter is larger than the outer diameter of the nozzle body 311, and the housing 312 covers the nozzle body 311 to provide a space between the nozzle body 311 and the housing 312. The ultrasonic nozzle 31 in this embodiment can allow the heat medium FL (antifreeze, etc.) to flow through the space, and the temperature of the nozzle body 311 can be adjusted as needed.

[0065] In the present embodiment, as described above, the nozzle body 311 can be heated by the heat medium FL, so that the blockage during freezing can be eliminated. In the particle manufacturing device 100 of the present embodiment that can discharge the raw material liquid L in a stable amount, it is possible to grasp whether the nozzle body 311 is blocked by monitoring the pressure of the containing space 10a. Therefore, the particle manufacturing device 100 of the present embodiment may include a pressure measuring instrument (not shown) for measuring the pressure of the containing space 10a. The ultrasonic nozzle 31 may be configured to adjust the temperature of the nozzle body 311 based on the measurement result of the pressure measuring instrument. The particle manufacturing device 100 of the present embodiment may be configured to heat the ultrasonic nozzle 31 when the pressure of the containing space 10a measured by the pressure measuring instrument reaches a certain reference value.

[0066] The mechanism for eliminating the blockage of the ultrasonic nozzle 31 may be different from the mechanism described above. As a mechanism for eliminating the blockage of the ultrasonic nozzle 31, for example, it is conceivable to provide a purge nozzle for removing the frozen object causing the blockage by blowing gas to the discharge port 31a of the ultrasonic nozzle 31. The purge gas blown from the purge nozzle to the ultrasonic nozzle 31 may be, for example, air or nitrogen. This purge gas may be supplied to the purge nozzle at room temperature, may be heated or supplied, or may be cooled. Blowing the purge gas to solve the blockage may be continuous or intermittent. When the purge gas is blown continuously, the blowing pressure may be constant, or the blowing pressure may be repeatedly increased and decreased.

[0067] The purge gas may be blown from the outside to the discharge port 31a, or may be supplied to the discharge port 31a through the flow channel 311b inside the nozzle. That is, when it is detected that the pressure of the raw material liquid L in the ultrasonic nozzle 31 is increasing, and the discharge port 31a or the flow channel 311b begins to be blocked by a frozen object or the like, the supply of the raw material liquid L may be stopped, and the purge gas may be supplied instead of supplying the raw material liquid L, and the frozen object or the like may be removed by the purge gas. Switching of the supply and stop of the purge gas or the like may be performed based on a reference value determined for the pressure of the accommodating space 10a.

[0068] The ultrasonic nozzle 31 in this embodiment can be as follows Figure 2C shown. Figure 2C The illustrated ultrasonic nozzle 31 includes a chamber 316 in which a discharge port 31 a opens. Figure 2CThe ultrasonic nozzle 31 shown includes a first chamber 316a and a second chamber 316b, wherein the first chamber 316a has an internal space for storing a raw material liquid L, applying ultrasonic vibration, and generating a granular raw material liquid L' due to the ultrasonic vibration, and the second chamber 316b has an internal space connected to the internal space of the first chamber 316b. In the ultrasonic nozzle 31, the internal space of the second chamber 316b adjacent to the accommodating space 10a is connected to the accommodating space 10a via the discharge port 31a.

[0069] The ultrasonic nozzle 31 is configured to supply the raw material liquid L to the first chamber 316a. The ultrasonic nozzle 31 has a liquid reservoir provided in the first chamber 316a for storing the raw material liquid L, so that the raw material liquid L always occupies a part of the internal space of the first chamber 316b, and the liquid level of the raw material liquid L is formed in the chamber. The ultrasonic nozzle 31 includes an ultrasonic vibrator 313 for applying ultrasonic vibration to the raw material liquid L stored in the liquid reservoir. The ultrasonic nozzle 31 is configured to generate a pressure difference between the accommodation space 10a and the space in the chamber 316 by evaporating water W from particles of the raw material liquid L protruding from the liquid level of the raw material liquid L stored in the liquid reservoir, and is configured so that the particles of the raw material liquid L enter the accommodation space 10a through the second chamber 316b and the discharge port 31a by using the pressure difference.

[0070] If the pressure difference alone is insufficient to transfer the particles of the raw material liquid L generated in the chamber 316 to the accommodation space 10a, for example, an airflow generating mechanism may be provided in the ultrasonic nozzle 31 to form an airflow in the chamber 316 toward the accommodation space 10a.

[0071] In the ultrasonic nozzle 31, water is evaporated at an early stage and the cooled raw material liquid L is discharged from the discharge port 31a, so the frozen particles A can be quickly formed in the accommodation space 10a. Figure 2C In the ultrasonic nozzle 31 shown, a mechanism for adjusting the temperature based on a reference value is preferably provided to prevent freezing in the liquid reservoir. Preferably, the particle manufacturing device 100 of this embodiment also includes a temperature adjustment device, which heats or cools the object to be processed to be discharged from the ultrasonic nozzle 31 when the object to be processed passes through the ultrasonic nozzle, and preferably, the temperature adjustment device can adjust the temperature based on the reference value, as shown below.

[0072] The ultrasonic nozzle 31 in this embodiment can be as follows Figure 2D shown. Figure 2D The ultrasonic nozzle 31 shown is Figure 2A or Figure 2C The ultrasonic nozzles 31 shown are common in that the ultrasonic nozzles 31 evaporate water W from the raw material liquid L and utilize the evaporation heat of the water W to cool the raw material liquid L to a frozen state. Figure 2DThe ultrasonic nozzle 31 shown is Figure 2C The ultrasonic nozzle 31 shown is common in that a chamber 316 is provided in which the discharge port 31a is open. Figure 2C The common features of the ultrasonic nozzles 31 shown are that the containing space 10a and the chamber 316 are connected to each other through the discharge port 31a, and the chamber 316 can be depressurized by the decompression device 20, and that the raw liquid L can be supplied to the chamber 316, and that water W can be evaporated from the raw liquid L in the chamber 316 to reduce the vacuum degree on the chamber 316 side to a level lower than the vacuum degree of the containing space 10a (to increase the air pressure in the chamber 316 to a level higher than the air pressure of the containing space 10a), thereby forming a water vapor flow from the chamber 316 toward the containing space 10a.

[0073] Figure 2D The ultrasonic nozzle 31 shown is a nozzle that freezes the raw material liquid L inside the ultrasonic nozzle 31 (inside the chamber 316 ). Figure 2D The illustrated ultrasonic nozzle 31 has an ultrasonic vibrator 313 disposed in a chamber 316 , and is configured to transmit vibrations of the ultrasonic vibrator 313 to a frozen object frozen in the chamber 316 . Figure 2D The illustrated ultrasonic nozzle 31 is configured to form frozen particles A within the ultrasonic nozzle 31 by pulverizing the frozen object through vibration.

[0074] The frozen particles A dispersed into the chamber 316 are discharged into the freezing chamber 10 together with the air flow (water vapor) carrying the moisture W discharged from the discharge port 31 a . Figure 2D The ultrasonic nozzle 31 shown is configured to introduce a carrier gas CG (such as nitrogen or air) into the chamber 316 so as to bias the A discharge of the frozen particles from the chamber 316. Specifically, Figure 2D The ultrasonic nozzle 31 shown includes an air supply pipe 317 opened in the chamber 316. The air supply pipe 317 is arranged so that the carrier gas CG can be introduced into the chamber 316. With such a configuration, Figure 2D The ultrasonic nozzle 31 shown can adjust the reduced pressure state in the chamber 316 (the degree of negative pressure acting on the raw material liquid). Figure 2D The ultrasonic nozzle 31 shown can use the carrier gas CG to be supplied from the air supply pipe 317 as the purge gas when the discharge port 31 a is blocked.

[0075] When the purge gas is supplied from the air supply pipe 317 to the chamber 316 in order to eliminate the clogging of the discharge port 31a, Figure 2A and Figure 2C Similar to the ultrasonic nozzle shown, the timing to start supply and the like can be appropriately set based on a reference value predetermined for the pressure of the accommodating space 10a.

[0076] For example, the reference value may be an absolute value (P2: P2<P1) set separately from the set value (P1) for normal operation. The reference value may be an amount of change in pressure in the accommodation space 10a over time.

[0077] In the former case, the reference value (P2) may be, for example, a value that is 50 Pa or more smaller than the set value (P1) for normal operation. The reference value (P2) may be a value that is 80 Pa or more smaller than the set value (P1), or may be a value that is 100 Pa or more smaller than the set value (P1).

[0078] In the latter case, a moving average value of the pressure in the accommodation space 10a that changes with time may be calculated, and a reference value (ΔPa (Pa / min)) of a decrease (ΔPa=(moving average value X minutes ago-current moving average value) / X minutes) of the moving average value within a predetermined time (e.g., within one minute) may be set. For example, the reference value (ΔPa) may be a value of 50Pa / min or more. The reference value may be 80Pa or more, or 100Pa or more.

[0079] The heat medium FL can be used not only for heating but also for cooling the nozzle body 311 or the raw liquid L. When the temperature of the raw liquid L is high and time is needed to freeze the raw liquid L after discharge, the raw liquid L can be cooled through the nozzle body 311, thereby easily forming frozen particles.

[0080] The particle manufacturing apparatus 100 of the present embodiment may include a liquid temperature measuring instrument (not shown) for measuring the temperature of the raw material liquid L. The ultrasonic nozzle 31 may be configured to adjust the temperature of the nozzle body 311 based on the measurement result of the liquid temperature measuring instrument.

[0081] like Figure 2A As shown, when the raw liquid L is discharged from the ultrasonic nozzle 31 into the freezing chamber 10 in a liquid state, the freezing of the raw liquid L depends on the vacuum degree of the freezing chamber 10, but freezing can generally occur near the discharge port 31a. When the freezing chamber 10 is over-depressurized, the raw liquid L is frozen before it is separated from the nozzle body 311 and becomes a particle form, and in the ultrasonic nozzle 31, the nozzle body 311 performs ultrasonic vibration at the discharge port 31a, so even if the raw liquid L is frozen, the raw liquid L is crushed by the vibration of the nozzle body 311. Therefore, in the ultrasonic nozzle 31, the discharge port 31a is prevented from being blocked, resulting in a state where no frozen particles A are formed. In the present embodiment, it is not necessary to strictly control the vacuum degree of the freezing chamber 10 in order to prevent blocking in the ultrasonic nozzle 31, and the frozen particles A can be easily prepared.

[0082] In the method of discharging the raw material liquid and forming frozen particles under the extremely low temperature environment, the cooling caused by sensible heat is mainly performed, so as the temperature of the discharged liquid decreases, the temperature difference with the ambient temperature becomes smaller, and the cooling rate will decrease. In the present embodiment, the cooling of the raw material liquid mainly includes the latent heat of water vaporization, so the raw material liquid will be quickly cooled immediately after the discharge. For example, the evaporation heat of water at 25°C is about 600 kcal / kg. If the specific heat of the raw material liquid L is 1cal / K similar to the specific heat of water, the temperature is reduced by about 30°C by evaporating only 5% of the water, and frozen particles will be formed. In the present embodiment, the ultrasonic nozzle is unlikely to be blocked due to freezing, so the interior of the freezing chamber 10 can be kept in a high vacuum to quickly freeze the raw material liquid. Therefore, in the present embodiment, the frozen particles are quickly formed, and the freeze-dried particles finally formed are also effectively prepared.

[0083] In the present embodiment, as described above, the particles of the raw liquid are frozen into solid frozen particles. The speed of discharging water from the frozen particles is generally slower than the speed of discharging water from the particles of the raw liquid before freezing. At a temperature close to the freezing point, the frozen particles may melt and may cause other frozen particles to adhere to each other, and may also cause agglomerates to appear. In addition, at a temperature close to the freezing point, the frozen particles tend to adhere to the wall surface of the freezing chamber 10 or the equipment in the room. Therefore, in the present embodiment, it is desired to reduce the temperature of the frozen particles more quickly.

[0084] The raw material liquid may contain an organic solvent to reduce the temperature of the frozen particles when freezing. The raw material liquid of this embodiment contains water. The boiling point of the organic solvent is lower than that of water, so when the particles are frozen, the organic solvent can be quickly discharged from the particles of the raw material liquid. In addition, when the freezing point of the organic solvent is lower than that of water, the rate of discharge of the organic solvent from the particles is less likely to decrease, even in the temperature range that reduces the discharge rate of water when the raw material liquid without organic solvent is frozen. Therefore, when the raw material liquid contains an organic solvent whose boiling point and freezing point are lower than those of water, excellent cooling performance due to evaporation heat is exhibited in a lower temperature range, and frozen particles that are less likely to melt can be formed. The raw material liquid containing an organic solvent is less likely to solidify, so freezing in the ultrasonic nozzle 31 is less likely to occur. Therefore, when a raw material liquid containing an organic solvent is used, the amount of raw material liquid discharged through the ultrasonic nozzle 31 per unit time is stable, and frozen particles with uniform particle size can be obtained. For example, the organic solvent may be an organic solvent whose boiling point and freezing point are lower than those of water at a constant pressure (1atm).

[0085] For example, the organic solvent described above may be a hydrophilic organic solvent having a solubility of 10 g / 100 g or more in water at room temperature and constant pressure (e.g., 23° C. and 1 atm), or may be a hydrophobic organic solvent having a solubility lower than that of a hydrophilic organic solvent. Examples of hydrophobic organic solvents include hexane, heptane, dichloromethane, 1,2-dichloroethane, trichloromethane, tetrachloroethane, triethylamine, diethyl ether, ethyl acetate, and methyl tert-butyl ether. Examples of hydrophilic organic solvents include tetrahydrofuran, methanol, ethanol, 1-propanol, 2-propanol, 2-butanol, acetone, and acetonitrile.

[0086] Preferably, the organic solvent contained in the raw material solution is a hydrophilic organic solvent, more preferably an alcohol solvent (such as ethanol) or acetonitrile, and even more preferably any one or both of ethanol and acetonitrile.

[0087] For example, the content of the organic solvent in the raw material solution can be 0.1 mass % (or 0.1% by mass) or higher. The content of the organic solvent can be 0.5 mass % or higher, 1 mass % or higher, 2 mass % or higher, or 5 mass % or higher. For example, the content of the organic solvent in the raw material solution can be 50 mass % or lower. The content of the organic solvent in the raw material solution can be 40 mass % or lower, or 30 mass % or lower.

[0088] When the content of water in the raw material liquid is 100 parts by mass (or 100 parts by mass), the content of the organic solvent in the raw material liquid can be, for example, 0.1 parts by mass or higher. Relative to 100 parts by mass of water, the content of the organic solvent can be 0.5 parts by mass or higher, 1 part by mass or higher, 2 parts by mass or higher, or 5 parts by mass or higher. For example, relative to 100 parts by mass of water, the content of the organic solvent in the raw material liquid can be 100 parts by mass or less. Relative to 100 parts by mass of water, the content of the organic solvent in the raw material liquid can be 50 parts by mass or less, 40 parts by mass or less, or 30 parts by mass or less. The raw material liquid containing an organic solvent can be used in other embodiments (the second embodiment, the third embodiment, and the fourth embodiment) described later. The advantages obtained by using a raw material liquid containing an organic solvent will also be shown in other embodiments.

[0089] In the present embodiment, a plurality of ultrasonic nozzles 31 are provided at one freezing chamber 10. Therefore, even if one ultrasonic nozzle 31 is clogged, frozen particles A can be continuously produced by other ultrasonic nozzles 31. In addition, in the present embodiment, the raw material liquid L to be discharged from one pump 32 is distributed to the plurality of ultrasonic nozzles 31, so when one ultrasonic nozzle 31 is clogged, the flow rate of the raw material liquid L in the other ultrasonic nozzles 31 increases, and the other ultrasonic nozzles 31 can be prevented from being clogged after the one ultrasonic nozzle 31. In addition, in the present embodiment, the ultrasonic vibrator 313 is arranged in front of the discharge port 31a, so that the raw material liquid L is heated by the heat generated by the ultrasonic vibrator 313 just before the raw material liquid L is discharged from the discharge port 31a. Therefore, even when the ultrasonic nozzle 31 is frozen and clogged once, the raw material liquid L increases in temperature inside the nozzle body 311 in the ultrasonic nozzle 31. Then, in the ultrasonic nozzle 31, the evaporation heat stops due to the clogging, and the temperature decreases. Therefore, even when the clogging due to freezing occurs once, the ultrasonic nozzle 31 can eliminate the clogging in a short time.

[0090] The particle manufacturing device 100 of the present embodiment includes a stirring device 40 for removing water from the frozen particles A while heating and stirring the frozen particles A under a reduced pressure environment. The particle manufacturing device 100 of the present embodiment also includes a reduced pressure drying chamber 50. The reduced pressure drying chamber 50 can be depressurized by a depressurizing device 20 for depressurizing the freezing chamber 10 or a depressurizing device different from the depressurizing device 20. In the present embodiment, the freezing chamber 10 and the reduced pressure drying chamber 50 are depressurized by one depressurizing device 20.

[0091] When a raw material liquid containing an organic solvent is used, the organic solvent can be recovered by exhausting the freezing chamber 10 or the reduced pressure drying chamber 50 in the path (exhaust path) for decompressing the freezing chamber 10 or the reduced pressure drying chamber 50. The recovery device (not shown) for recovering the organic solvent may be a condenser for freezing and recovering the organic solvent. Specifically, for example, the exhaust path may be provided with a condenser including a heat exchanger capable of cooling the gas to be discharged from the freezing chamber 10 or the reduced pressure drying chamber 50 to a temperature equal to or lower than the freezing point of the organic solvent. When the organic solvent is hydrophilic, the cooling temperature of the heat exchanger does not need to be equal to or lower than the freezing point of the organic solvent, and by providing a heat exchanger capable of adjusting the temperature to be lower than the freezing point of the mixed liquid containing water and the organic solvent, the organic solvent contained in the exhaust gas can be frozen together with water and adhered to the surface of the heat exchanger. The organic solvent can recover the adhered material in a frozen state or recover after the adhered material is melted.

[0092] The reduced pressure drying chamber 50 is used to dry the frozen particles A to form freeze-dried particles. The reduced pressure drying chamber 50 has a storage space 50a that can accommodate the frozen particles A manufactured in the freezing chamber 10. The reduced pressure drying chamber 50 is located below the freezing chamber 10 and is connected to the freezing chamber 10 in the up and down directions. The reduced pressure drying chamber 50 is connected to the freezing chamber 10 via an opening and closing device 60, and is configured so that when the opening and closing device 60 is in an open state, the storage space 50a is communicated with the storage space 10a of the freezing chamber 10. When the opening and closing device 60 is in a closed state, the storage space 50a is in a sealed state, and the reduced pressure drying chamber 50 can be decompressed to a predetermined vacuum degree by the decompression device 20.

[0093] The stirring device 40 in the particle production device 100 of the present embodiment is configured to stir the frozen particles A transferred from the freezing chamber 10 to the reduced pressure drying chamber 50. The stirring device 40 in the present embodiment is configured to stir the frozen particles A in the reduced pressure drying chamber 50.

[0094] The reduced pressure drying chamber 50 includes a vertical cylindrical main body portion 51 and a cover portion 52, the cover portion closing the upper opening of the main body portion 51. The diameter of the main body portion 51 decreases toward the bottom 51d, and the overall shape of the internal space is conical. In other words, the main body portion 51 of the present embodiment has a side wall surface 51w, the diameter of which increases upward and outward from the peripheral edge of the bottom portion 51d, and the peripheral edge of the bottom portion 51d defines the lower end of the internal space. The main body portion 51 of the present embodiment itself has a conical shape.

[0095] The reduced pressure drying chamber 50 is arranged in the particle manufacturing device 100 so that the central axis 51c of the main body 51 is in the vertical direction. That is, the height direction H of the reduced pressure drying chamber 50 in this embodiment is the direction in which the central axis 51c extends. The radial direction D of the reduced pressure drying chamber 50 in this embodiment refers to the horizontal direction passing through the central axis 51c.

[0096] The reduced pressure drying chamber 50 has two openings formed in the cover portion 52. One opening is an exhaust port 52a, and the other opening is a supply port 52b for frozen particles A. A filter unit 53 is connected above the exhaust port 52a. The reduced pressure drying chamber 50 is configured to exhaust air via the filter unit 53 when the accommodating space 50a is exhausted by the decompression device 20. The opening and closing device 60 is connected above the supply port 52b. The reduced pressure drying chamber 50 is configured so that the frozen particles A falling from the freezing chamber 10 due to gravity by bringing the opening and closing device 60 into an open state are accommodated in the main body portion 51 through the supply port 52b. In the present embodiment, the freezing chamber 10 may be provided with a filter unit, and the filter unit may be arranged in the middle of the exhaust path from the reduced pressure drying chamber 50 or the freezing chamber 10 to the decompression device 20.

[0097] The main body portion 51 is double-walled except for the two end portions in the height direction H, and has a jacket portion 511 through which a heat medium can flow. That is, the reduced pressure drying chamber 50 of the present embodiment is provided with a heat transfer surface 50b for heating or cooling the contained object in the main body portion 51, and can adjust the temperature of the contained frozen particles A. The bottom portion 51d of the main body portion 51 is provided with a discharge port 51a for discharging freeze-dried particles obtained by drying the frozen particles A in a frozen state.

[0098] The exhaust port 52a and the supply port 52b are arranged on the left and right sides, respectively, and the central part of the cover part 52 is between the left and right sides. The rotating shaft 41 of the stirring device 40 is inserted in the central part of the cover part 52. The upper end portion of the rotating shaft 41 extends above the cover part 52 and is accommodated in the gear box 42 arranged above the cover part 52. The rotating shaft 41 passes through the cover part 52 and extends downward to pass through the central part of the accommodating space 50a. That is, the rotating shaft 41 extends in the vertical direction along the central axis 51c of the main body part 51 having a conical shape. The lower end portion of the rotating shaft 41 is not connected to the bottom of the main body part 51, and is located slightly above the bottom of the main body part 51 as a free end.

[0099] The stirring device 40 includes a rotating mechanism 43 for rotating the gear of the gear box 42 so that the rotating shaft 41 rotates around the axis by the driving force of the rotating mechanism 43. The stirring device 40 includes a rotating shaft 41 as a rotating body and a stirring blade 44 fixed to the rotating shaft 41, and the rotating shaft is used to rotate in the reduced pressure drying chamber 50 to stir the frozen particles A. The stirring device 40 includes a spiral belt-shaped blade 441, which rotates at the lower end portion of the main body part 51, and a plurality of paddles 442, which rotate at the center portion in the height direction of the main body part 51. The stirring device 40 is configured to stir the frozen particles A transferred from the freezing chamber 10 and accommodated in the accommodation space 50a by the spiral belt-shaped blade 441 or the paddle 442.

[0100] In the stirring device 40 of the present embodiment, when the rotating body rotates, the rotating shaft 41 extends along the axial center, and the rotating body only rotates. The rotating body may be a scraper that circulates along the heat transfer surface 50b of the reduced pressure drying chamber 50 in the reduced pressure drying chamber 50. That is, the rotational motion of the rotating body in the reduced pressure drying chamber 50 may be a rotation around the axial center or a revolution around the axial center. In addition, the stirring device 40 may circulate along the wall of the reduced pressure drying chamber 50 while rotating the rotating shaft to which the stirring blade is attached, or may include a rotating body that can rotate by combining rotation and revolution.

[0101] In the particle manufacturing device 100 of the present embodiment, water removal from the raw material liquid L used to form freeze-dried particles can be performed in two stages (i.e., in the freezing chamber 10 and the reduced pressure drying chamber 50), and the drying conditions in the freezing chamber 10 and the drying conditions in the reduced pressure drying chamber 50 can be adjusted separately.

[0102] When the freezing chamber 10 is over-depressurized, the ultrasonic nozzle 31 may be clogged, but there is no such problem in the reduced pressure drying chamber 50, so the frozen particles A can be dried at a higher vacuum degree in the reduced pressure drying chamber 50 than in the freezing chamber 10, and water can be removed from the frozen particles A by sublimation. In addition, by heating the frozen particles A by raising the temperature of the inner wall surface of the main body part 51, the drying of the frozen particles A can be promoted. Therefore, the moisture content of the freeze-dried particles obtained by drying in the reduced pressure drying chamber 50 can be significantly lower than the moisture content of the frozen particles A obtained by freezing in the freezing chamber 10. In addition, by performing stirring by the stirring blade 44 in the reduced pressure drying chamber 50, the removal of water from the frozen particles A is promoted.

[0103] In the particle manufacturing device 100 of the present embodiment, the spiral ribbon blade 441 or the paddle 442 moves in the accommodation space 50a so as to scrape the frozen particles A from the heat transfer surface 50b during the rotation of the rotating shaft 41. Therefore, in the particle manufacturing device 100 of the present embodiment, further drying of the frozen particles A is promoted, and the dry state of the obtained freeze-dried particles can be made relatively uniform. In the particle manufacturing device 100 of the present embodiment, the rotating shaft 41 or the stirring blade 44 can also be controlled in terms of temperature, so that the above-mentioned effect can be more significantly exhibited.

[0104] In the method for manufacturing frozen particles using the particle manufacturing device 100 of the present embodiment, frozen particles obtained by freezing a raw material liquid L in the form of particles are manufactured by performing the following steps: a step of decompressing the raw material liquid L containing moisture as an object to be processed, a step of cooling and freezing the raw material liquid L by evaporating the moisture, and a step of forming the frozen raw material liquid L or the raw material liquid L before freezing into a particle form by an ultrasonic nozzle.

[0105] In one aspect of the present invention applied to a method for manufacturing frozen particles, a raw liquid L (which is a liquid object to be processed containing moisture) is discharged from an ultrasonic nozzle 31 into a receiving space 10a of a freezing chamber 10 that has been decompressed, and the raw liquid L is frozen due to evaporation of moisture to form frozen particles in the receiving space 10a. In another aspect of the present invention applied to a method for manufacturing frozen particles, the raw liquid L is supplied to an ultrasonic nozzle 31 whose internal space is in a decompressed state, and the raw liquid L is decompressed and frozen inside or on a surface of the ultrasonic nozzle 31. In the method for manufacturing frozen particles, the raw liquid L is formed into a particle form inside or on a surface of the ultrasonic nozzle 31 by ultrasonic vibration to form frozen particles A, and the formed frozen particles A are discharged from the ultrasonic nozzle 31 into the freezing chamber 10.

[0106] In the method of manufacturing frozen particles using the particle manufacturing device 100 of the present embodiment, freeze-dried particles are manufactured by performing a step of drying frozen particles A obtained by freezing under reduced pressure in a reduced pressure drying chamber 50 under a reduced pressure environment, and in the drying step, the frozen particles A are stirred in the reduced pressure accommodating space 50a as described above.

[0107] Preferably, the freeze-dried particles are dried to such an extent that the particles become a sufficiently dry solid at room temperature (e.g., 23° C.), and the frozen particles A may not be in a solid state at room temperature, for example, may be in a paste state (semi-solid state) at room temperature, or may be in a dry state sufficient to be restored to a liquid. In particular, the frozen particles A may be dried so that moisture can be removed to such an extent that the raw material liquid L becomes a concentrated liquid at room temperature.

[0108] For example, the freeze-dried particles are prepared so that the moisture content is 5% by mass or less. The moisture content of the freeze-dried particles can be 4% by mass or less, or 3% by mass or less. For example, the moisture content of the freeze-dried particles can be determined by dividing the change in mass of the freeze-dried particles dried in a gear oven at 105°C for 2 hours by the original mass of the freeze-dried particles.

[0109] When producing frozen particles A, first, the opening and closing device 60 is closed, and the freezing chamber 10 is evacuated by the vacuum pump 21, thereby reducing the pressure of the accommodation space 10a to atmospheric pressure or lower. The raw material liquid L may be pre-cooled so as to be easily frozen in the freezing chamber 10, for example, pre-cooled to a temperature of 0°C to 15°C.

[0110] For example, the freezing chamber 10 in which the frozen particles A are manufactured is adjusted so that, when the raw material liquid L is discharged, the accommodating space 10a has a pressure (absolute pressure) of 100Pa to 1000Pa. Preferably, the accommodating space 10a of the freezing chamber 10 is maintained within the above range until the discharge of a predetermined amount of the raw material liquid L is completed, and a predetermined amount of frozen particles A is stored in the freezing chamber 10. The lower pressure in the accommodating space 10a is conducive to freezing. The pressure is preferably 800Pa or less, more preferably 600Pa or less, and more preferably 400Pa or less. On the other hand, when the pressure is too low, the ultrasonic nozzle 31 may be clogged. Therefore, the pressure is preferably 150Pa or more, and more preferably 200Pa or more.

[0111] The pressure in the accommodating space 10a does not need to be constant from the start of manufacturing of the frozen particles A to the completion of manufacturing. For example, the pressure can be changed within a range that does not cause excessive changes in the size of the frozen particles A. For example, during the period from the start of manufacturing of the frozen particles to the completion of manufacturing, a pressure difference can be provided so that the difference from the minimum pressure to the maximum pressure is 10Pa or more and 100Pa or less, and the pressure can be repeatedly increased and decreased. Therefore, the nozzle body 311 can be prevented from being continuously and strongly cooled, and frozen particles can be manufactured while preventing the ultrasonic nozzle 31 from being blocked.

[0112] When a predetermined amount of frozen particles are stored in the freezing chamber 10, the discharge of the raw material liquid L is stopped, the opening and closing device is switched from the closed state to the open state, and the frozen particles A are transferred from the freezing chamber 10 to the reduced pressure drying chamber 50. In the reduced pressure drying chamber 50, the transferred frozen particles A are slowly heated while being stirred to remove moisture. For example, the heating of the frozen particles A can be performed by gradually increasing the temperature of the heat medium flowing through the jacket. The reduced pressure drying chamber 50 is adjusted so that when the frozen particles A are dried while being stirred, the accommodation space 50a has a pressure (absolute pressure) of 1Pa to 100Pa. The accommodation space 50a is adjusted to a predetermined temperature in the range of, for example, -40°C to 40°C by the jacket portion 511 arranged on the wall surface. The pressure of the accommodation space 50a or the temperature of the wall surface can be started before or after the frozen particles A are transferred.

[0113] When the freezing chamber 10 is evacuated by the vacuum pump 21, the reduced pressure drying chamber 50 can be evacuated together. When the frozen particles A are dried in the reduced pressure drying chamber 50 to form freeze-dried particles, the next batch of frozen particles A can be manufactured in the freezing chamber 10. That is, in the present embodiment, the frozen particles A can be manufactured in a batch manner, wherein the following drying step is performed, wherein a raw material liquid L (which is a liquid object to be processed containing moisture) is discharged from the ultrasonic nozzle 31 into a first space that has been decompressed, and frozen particles A are formed in the first space by freezing the discharged raw material liquid L due to evaporation of moisture, and then the frozen particles A are transferred to a second space different from the first space and dried in the second space. During the drying step being performed, the next batch of frozen particles A can be prepared in the first space. Drying of the frozen particles A can be started after a plurality of batches of frozen particles A are accommodated in the reduced pressure drying chamber 50.

[0114] The method of manufacturing frozen particles using the particle manufacturing apparatus 100 of the present embodiment includes a drying step of drying the frozen particles A obtained by freezing the discharge from the ultrasonic nozzle 31 in the reduced pressure drying chamber 50 to manufacture freeze-dried particles, and the drying step includes stirring the frozen particles A in the reduced pressure accommodation space 50a. Therefore, in the present embodiment, sufficiently dried freeze-dried particles can be easily obtained.

[0115] In the particle manufacturing device 100 of the present embodiment, an aspect of setting the stirring device 40 in the reduced pressure drying chamber 50 is shown, and for example, the freezing chamber 10 may also be provided with a stirring device similar to the reduced pressure drying chamber 50 or a stirring device different from the reduced pressure drying chamber 50, and the stirring device stirs the frozen particles A to prevent the formation of agglomerates that aggregate a plurality of frozen particles A. In addition, in the case where the wall surface of the freezing chamber 10 is cooled to cool the frozen particles A, a cooling effect can be applied to a larger number of frozen particles A by stirring the frozen particles A. In the particle manufacturing device 100 or the method for manufacturing frozen particles according to the present embodiment, various modifications may be appropriately made in addition to these matters. The specific examples of the particle manufacturing device 100 or the method for manufacturing frozen particles described above may be appropriately used in the particle manufacturing device or the method for manufacturing frozen particles according to the following embodiments. Therefore, a detailed description related to the characteristics exhibited by the device or the method for using the device may not be repeated below.

[0116] (Second embodiment)

[0117] Various modifications may be made to the particle manufacturing apparatus 100 of the above example. FIG. 3A to FIG. 3D , Figure 4A and Figure 4B A particle production apparatus according to a second embodiment is described.

[0118] In the particle manufacturing apparatus 100 of the first embodiment, the freezing chamber 10 and the reduced pressure drying chamber 50 are separate chambers, while in the second embodiment, the freezing chamber 10 is also used as the reduced pressure drying chamber 50, and the freezing chamber 10 of the second embodiment is configured not only to form frozen particles A from the raw material liquid L, but also to dry the formed frozen particles under reduced pressure to form freeze-dried particles. That is, the particle manufacturing apparatus 101 of the second embodiment is different from the particle manufacturing apparatus 100 of the first embodiment in that the reduced pressure drying chamber 50 of the first embodiment is used as the freezing chamber 10, and freezing and drying are both performed in the freezing chamber 10.

[0119] The particle manufacturing device 101 of the second embodiment uses the reduced pressure drying chamber 50 of the first embodiment as the freezing chamber 10, so the freezing chamber 10 has the same shape as the reduced pressure drying chamber 50 in the first embodiment. That is, the freezing chamber 10 includes a main body portion 11 and a cover portion 12, the main body portion 11 has a vertical long cone, and the cover portion closes the upper opening of the main body portion 11. The cover portion 12 is provided with an exhaust port 12a. The main body portion 11 is similar to the reduced pressure drying chamber 50 of the first embodiment in that the main body portion 11 has a side wall surface 11w that rises outward from the bottom portion 11d of the main body portion and an internal space having a conical shape.

[0120] The cover portion 12 of the particle manufacturing device 101 of the second embodiment has the same shape as the cover portion 52 of the reduced pressure drying chamber 50 of the first embodiment. The cover portion 12 has a cover body 120 that covers the upper opening of the main body portion 11. The cover body 120 is provided with two openings, the first opening being an exhaust port 12a for performing exhaust through the filter unit 13 (similar to the exhaust port 52a of the first embodiment). The second opening is a supply port 12b for supplying particles formed by the ultrasonic nozzle 31 to the accommodating space 10a.

[0121] The cover portion 12 of the present embodiment includes two cylinders (a first cylinder 121 and a second cylinder 122) extending upward from the cover body 120. The lower end portion of the first cylinder 121 is used as an exhaust port 12a and is used to connect to the filter unit 13. The lower end portion of the second cylinder 122 is used as a supply port 12b and is used to fix the ultrasonic nozzle 31.

[0122] When viewed from above, the cover body 120 of the present embodiment has a circular plate shape. The cover body 120 has a circular plate shape that is larger than the upper opening of the main body part 11. When viewed from a horizontal direction, the cover body 120 has a dome shape. The cover body 120 includes a dome portion 120a that protrudes upward and an outer edge portion 120b that extends outward from the outer peripheral edge of the dome portion 120a. When the cover part 12 is viewed from a horizontal direction, the dome portion 120a of the cover body 120 has a shape that protrudes upward from the outer edge portion 120b. The dome portion 120a has a shape that becomes higher from the outer edge portion 120b toward the center portion of the cover body 120. The cover body 120 is attached to the main body part 11 by making the outer edge portion 120b contact with the upper end portion of the main body part 11 from above.

[0123] The first cylinder 121 and the second cylinder 122 are separately arranged on the left and right sides of the cover body 120. Figure 3A In the example shown, the first cylinder 121 is disposed on the left side of the cover body 120, and the second cylinder 122 is disposed on the right side of the cover body 120. The first cylinder 121 and the second cylinder 122 extend upward from the dome portion 120a, respectively. Therefore, the exhaust port 12a and the supply port 12b are each disposed in the middle from the center of the cover portion 12 to the outer edge portion 120b.

[0124] The upper end of the accommodation space 10a in this embodiment is defined by the lower surface of the cover portion 12 (the lower surface 120s of the dome portion 120a). The ultrasonic nozzle 31 in this embodiment protrudes inward from the lower surface 120s of the dome portion 120a. That is, the distal end portion of the ultrasonic nozzle 31 protrudes from the supply port 12b located at the lower end edge of the second cylindrical body 122 and enters the accommodation space 10a.

[0125] When cut along a horizontal plane, the accommodation space 10a in this embodiment has a circular shape. When the horizontal plane is set to pass through the portion where the main body portion 11 and the cover portion 12 contact each other, the area of ​​the circular region is the largest. That is, the size of the accommodation space 10a in the radial direction D is the largest at the portion where the main body portion 11 and the cover portion 12 contact each other.

[0126] The ultrasonic nozzle 31 in this embodiment is located above the position where the accommodating space 10a has the maximum diameter, and the discharge direction of the object to be processed is downward. When a virtual axis Xn extending from the ultrasonic nozzle 31 along the discharge direction of the object to be processed is set, the lower surface of the cover portion 12 expands in a direction orthogonal to the virtual axis Xn in the peripheral portion of the supply port 12b. That is, when the position where the ultrasonic nozzle 31 is set is taken as the starting point, the lower surface of the cover portion 12 (which defines the upper end of the accommodating space 10a) expands in a direction away from the virtual axis Xn. The lower surface of the cover portion 12 continues to move away from the virtual axis Xn until the lower surface reaches the position where the accommodating space 10a has the maximum diameter.

[0127] As described above, in the present embodiment, the ultrasonic nozzle 31 is arranged above a position where the discharge direction of the object to be processed is downward and the accommodating space 10a has a maximum diameter, the freezing chamber 10 has an inner wall surface defining the upper edge of the accommodating space 10a, the distal end portion of the ultrasonic nozzle 31 protrudes from the inner wall surface, and the inner wall surface is formed to continue to move away from the virtual axis Xn from the position where the ultrasonic nozzle 31 is set until the inner wall surface reaches the position where the accommodating space 10a has a maximum diameter, and the virtual axis Xn extends from the ultrasonic nozzle 31 in the discharge direction of the object to be processed.

[0128] In such Figure 2A In the ultrasonic nozzle 31 shown, when the direction of the extension line extending from the discharge port 31a until reaching the discharge port 31a while maintaining the flow direction of the object to be processed is taken as the discharge direction of the object to be processed, the holding portion (flange portion 3111) vibrates in the discharge direction and also vibrates in the direction orthogonal to the discharge direction. Figure 2A In the ultrasonic nozzle 31 shown, a portion of the particles can also be discharged in a direction close to a right angle with respect to the discharge direction of the object to be processed. In the present embodiment, preferably, the distal end portion of the ultrasonic nozzle 31 protrudes from the supply port 12b, and the holding portion is located in the accommodating space 10a. In this case, even if the particles are discharged in the lateral direction, the moving direction of the particles is substantially parallel to the lower surface of the cover portion 12, and the particles can be prevented from adhering to the peripheral portion of the supply port 12b, etc. By the way, by making the distal end portion of the ultrasonic nozzle 31 protrude from the supply port 12b, the particles can be prevented from adhering to the peripheral portion of the supply port 12b, which is not only applicable to Figure 2A The ultrasonic nozzle 31 shown is also applicable to other types of ultrasonic nozzles.

[0129] The particle manufacturing device 101 of this embodiment is similar to the particle manufacturing device 100 of the first embodiment in that the raw material liquid may contain a predetermined proportion of organic solvent. In this case, a recovery device for recovering the organic solvent may be arranged.

[0130] The freezing chamber 10 of the second embodiment is similar to the reduced pressure drying chamber 50 of the particle manufacturing apparatus 100 of the first embodiment in that the filter unit 13 is connected above the exhaust port 12 a and the accommodation space 10 a is exhausted through the filter unit 13 by the reduced pressure device 20 .

[0131] In the present embodiment, the exhaust port 12a and the ultrasonic nozzle 31 are both provided in the cover portion 12 constituting the upper portion of the freezing chamber 10. Figure 3A and Figure 3B As shown, the exhaust port 12a and the ultrasonic nozzle 31 are arranged separately on the left and right sides of the freezing chamber 10. For example, the exhaust port 12a and the ultrasonic nozzle 31 are arranged at positions opposite to each other relative to the center (central axis 10c) of the freezing chamber 10 when viewed from above. The particles of the raw liquid L are discharged downward from the ultrasonic nozzle 31, so by arranging the ultrasonic nozzle 31 in the upper part of the freezing chamber 10, the time during which the raw liquid L can fall can be extended. On the other hand, when the time during which the particles of the raw liquid L drift in the accommodation space 10a of the freezing chamber 10 becomes longer, the raw liquid L may be discharged to the outside from the exhaust port 12a, or may be sucked back into the filter unit 13 to cause clogging of the filter. When the exhaust port 12a is arranged at the bottom, the possibility of this situation increases, so in the present embodiment, the exhaust port 12a is also arranged at the upper part of the freezing chamber 10. The distance in the horizontal direction from the end edge of the exhaust port 12a to the discharge port 31a of the ultrasonic nozzle 31 is preferably 30 cm or more, and more preferably 50 cm or more.

[0132] The ultrasonic nozzle 31 in the present embodiment is arranged on the cover part 12 so that the discharge port 31a is located at the lower end. The ultrasonic nozzle 31 can be arranged so that when the freezing chamber 10 is viewed from the horizontal direction, the discharge port 31a is higher than the exhaust port 12a. Preferably, the particle manufacturing device 100 of the present embodiment includes an ultrasonic nozzle 31 at which the discharge port 31a is arranged at the same height as the exhaust port 12a or at a position lower than the exhaust port 12a.

[0133] When the wall surface defining the upper edge of the accommodating space 10a has a surface inclined relative to the horizontal plane, and the exhaust port 12a is open at the inclined surface, the position in the height direction H may be different between one position and another position of the opening edge of the exhaust port 12a. In this case, the exhaust port 12a includes an uppermost portion having the highest position in the height direction H, a lowermost portion having the lowest position in the height direction H, and a middle portion located at the midpoint from the lowermost portion to the uppermost portion. In this case, the "position of the exhaust port 12a" refers to the "position of the uppermost portion". In this case, more preferably, the particle manufacturing device 100 includes an ultrasonic nozzle 31 in which the discharge port 31a is arranged at a position lower than the middle portion of the exhaust port 12a. More preferably, the particle manufacturing device 100 includes an ultrasonic nozzle 31 in which the discharge port 31a is arranged at a position lower than the lowest portion of the exhaust port 12a.

[0134] When a plurality of ultrasonic nozzles 31 are provided, the positions in the height direction H may be different between the discharge port 31a of one ultrasonic nozzle 31 and the discharge port 31a of another ultrasonic nozzle 31 among the plurality of ultrasonic nozzles 31. In this case, the number of ultrasonic nozzles 31 whose discharge ports 31a are arranged at a position lower than the exhaust port 12a may be only one, two or more, or all of the ultrasonic nozzles 31. When the exhaust port 12a has an uppermost portion, a middle portion, and a lowermost portion, the number of ultrasonic nozzles 31 whose discharge ports 31a are arranged at a position lower than the middle portion may be only one, two or more, or all of the ultrasonic nozzles 31. The number of ultrasonic nozzles 31 whose discharge ports 31a are arranged at a position lower than the lowest portion may be only one, two or more, or all of the ultrasonic nozzles 31.

[0135] The freezing chamber 10 of the second embodiment is similar to the reduced pressure drying chamber 50 of the first embodiment in that the main body part 11 has a jacket part 111, a heat transfer surface 10b for heating or cooling the contained object is arranged in the main body part 51, and the temperature of the contained frozen particles A can be adjusted.

[0136] The particle manufacturing device 101 of the second embodiment is the same as the particle manufacturing device of the first embodiment in the configuration or arrangement of the stirring device 40. That is, in the particle manufacturing device 101 of the second embodiment, the stirring device 40 is provided with a rotating body arranged in the freezing chamber 10 and including a rotating shaft 41 or a stirring blade 44, as a rotating body rotating around an axial center passing through the freezing chamber 10, and the frozen particles A contained in the freezing chamber 10 are stirred by the rotation of the stirring blade 44.

[0137] In the first embodiment, the frozen particles are formed by the ultrasonic nozzle 31 in the freezing chamber 10, which is the antechamber of the reduced pressure drying chamber 50 including the rotating shaft 41 or the stirring blade 44. On the other hand, in the particle manufacturing device 101 of the second embodiment, the distal end portion of the ultrasonic nozzle 31 is located in the accommodation space 10a accommodating the rotating shaft 41 or the stirring blade 44, rather than in the antechamber. That is, in the particle manufacturing device 101 of the second embodiment, the ultrasonic nozzle 31 discharges particles directly into the accommodation space 10a accommodating the rotating shaft 41 or the stirring blade 44.

[0138] like Figure 3A and Figure 3B As shown, in the second embodiment, as in the first embodiment, a plurality of ultrasonic nozzles 31 are provided in the cover portion 12. Figure 3A and Figure 3B As shown, the plurality of ultrasonic nozzles 31 may be arranged along the radial direction D of the main body portion 11, or as shown in FIG. Figure 3C and Figure 3D As shown, they can be arranged along the circumferential direction R of the main body portion 11. Figure 3C As shown, when a virtual line Rx extending horizontally from the center of the freezing chamber 10 to the center of the exhaust port 12a is defined as a starting point, and the direction of the virtual line Rx rotating clockwise around the central axis 10c of the freezing chamber 10 is defined as a normal rotation direction (positive direction: +θ), a plurality of ultrasonic nozzles 31 are preferably arranged within a predetermined range.

[0139] In the top view of the freezing chamber 10, the position of the ultrasonic nozzle 31 (the position of the discharge port 31a) can be within the range of 90° or more and 270° or less, within the range of 120° or more and 240° or less, within the range of 135° or more and 225° or less, or can be substantially 180° relative to the position of the exhaust port 12a (the center position) in the clockwise direction.

[0140] When a plurality of ultrasonic nozzles 31 are provided, all ultrasonic nozzles 31 are preferably arranged within the above range. That is, when the freezing chamber 10 is viewed from the horizontal direction so that the exhaust port 12a is located at the leftmost position, the plurality of ultrasonic nozzles 31 are preferably arranged within the range from the center of the freezing chamber 10 to the right end.

[0141] As described above, in the present embodiment, the cross-sectional shape of the accommodating space 10a is circular in a horizontal plane passing through the portion where the main body portion 11 and the cover portion 12 are in contact with each other. The circle defining the outer peripheral edge of the accommodating space 10a at this portion has the maximum diameter in the cross-sectional shape of the accommodating space 10a. The ultrasonic nozzle 31 in the present embodiment is arranged above a position where the discharge direction of the object to be processed is downward and the accommodating space 10a has the maximum diameter. The distal end portion of the ultrasonic nozzle 31 is located between the center of the cover portion 12 and the outer edge portion 120b. Therefore, the circle defining the cross-sectional shape of the accommodating space 10a at the position where the accommodating space 10a has the maximum diameter is defined as a virtual circle Cn, and the shape drawn by the virtual line Ln extending from each point on the circumference of the virtual circle Cn to the distal end portion of the ultrasonic nozzle 31 is not a right cone, but rather is a shape such as Figure 3E The oblique cone shown.

[0142] As described above, the ultrasonic nozzle 31 of the present embodiment is arranged so that the distal end portion (e.g., the holding portion) protrudes from the supply port 12b. Preferably, the cover portion 12 in the present embodiment has a shape in which the lower surface 120s of the dome portion 120a does not intersect with the oblique cone. In other words, preferably, the ultrasonic nozzle 31 protrudes from the supply port 12b so that the line segment extending from the distal end portion toward each point on the virtual circle Cn is not blocked by the cover portion 12.

[0143] As described above, when the virtual line Ln extends from the distal end portion of the ultrasonic nozzle 31 toward each point on the circle (virtual circle Cn) that defines the outer peripheral edge of the accommodating space 10a at the portion where the accommodating space 10a has the largest diameter, the ultrasonic nozzle 31 is arranged so that the virtual line Ln is not blocked by the cover portion 12, and the distal end portion of the ultrasonic nozzle 31 is arranged in such an open space, whereby the frozen particles A can be prevented from adhering to the cover portion 12. When the particle manufacturing device 101 includes a plurality of ultrasonic nozzles 31, the number of ultrasonic nozzles 31 whose distal ends protrude in this manner may be only one, two or more, or all of the ultrasonic nozzles 31.

[0144] In the present embodiment, frozen particles A are prepared in a space where the stirring blade 44 is arranged. In the present embodiment, preferably, the height of the stirring blade 44 is set low so that the raw material liquid L reaches the stirring blade 44 before being sufficiently frozen and does not adhere to the stirring blade 44 because the raw material liquid L is discharged in the form of particles from the ultrasonic nozzle 31 arranged in the upper part of the freezing chamber 10. Preferably, the upper end of the stirring blade 44 is arranged at a position of 60% or less of the volume of the reduced pressure drying chamber 50, and preferably, at a position of 50% or less of the volume. That is, in the present embodiment, when the volume in the reduced pressure drying chamber 50 is accumulated from the bottom part, the upper end of the stirring blade 44 is preferably lower than a line that makes the cumulative value 60% of the total volume of the reduced pressure drying chamber 50, or a line that makes the cumulative value 50% of the total volume. More specifically, the upper end of the stirring blade 44 is preferably set at 30 cm or more below the discharge port 31 a of the ultrasonic nozzle 31, and more preferably, at 50 cm or more below the discharge port 31 a of the ultrasonic nozzle 31.

[0145] During operation of the stirring device 40, the stirring blade 44 moves greatly, while the rotating shaft 41 only rotates around the axis and does not change much compared to the stopped state. During operation, frozen particles are more likely to adhere to the rotating shaft 41 located at the same position than the stirring blade 44 moving around the rotating shaft 41. Frozen particles attached to the rotating shaft 41 are less likely to fall off than frozen particles attached to the stirring blade 44. Therefore, if Figure 4A As shown, when the ultrasonic nozzle 31 is arranged near the rotating shaft 41 to discharge the raw material liquid, the frozen particles may adhere to the rotating shaft 41 to form an agglomerate AB.

[0146] exist Figure 4B In the aspect shown, the ultrasonic nozzle for discharging the raw material liquid in the form of particles into the freezing chamber 10 discharges the raw material liquid from the upper part to the lower part of the freezing chamber 10. The rotating shaft 41 and the stirring blade 44 attached to the rotating shaft 41 are arranged in the accommodating space 10a of the freezing chamber 10 as a rotating body for stirring the frozen particles accommodated in the accommodating space 10a, and the rotating shaft 41 extends through the central part of the accommodating space 10a in the height direction H. The discharge direction DX of the raw material liquid from the ultrasonic nozzle 31 is a direction approaching the rotating shaft 41 as the raw material liquid travels to the lower part of the main body 11. However, the ultrasonic nozzle 31 is set so that the discharge direction DX does not intersect with the rotating shaft 41. Therefore, in Figure 4B In the illustrated aspect, frozen particles are prevented from adhering to the rotating shaft 41. The discharge direction DX of the raw material liquid refers to a direction extending from the discharge port 31a while maintaining the flow direction of the raw material liquid (object to be processed) until reaching the extended line of the discharge port 31a.

[0147] The discharge direction DX from the ultrasonic nozzle 31 toward the bottom portion 11d of the main body portion 11 may be set along the conical side wall surface 11w, or may be set parallel to the side wall surface 11w while maintaining a predetermined distance (e.g., 50 mm to 300 mm). When viewed from the direction of the central axis 10c, the discharge direction DX may be inward in the radial direction D (center direction), such as Figure 3C As shown, or it can be a direction inclined relative to the radial direction D, such as Figure 3D shown.

[0148] In the present embodiment, it is also conceivable that the raw liquid L is frozen on the surface of the stirring blade 44, so that the frozen object remains attached to the stirring blade 44. In this case, a purification nozzle that is the same as the purification nozzle used to eliminate the clogging of the discharge port 30a can be provided to remove the frozen object adhering to the stirring blade 44. In the present embodiment, the frozen particles A may not be formed in the freezing chamber 10, but may be formed inside or on the surface of the ultrasonic nozzle 31. In this case, after the raw liquid L is turned into the frozen particles A, the frozen particles A are discharged into the freezing chamber 10, which prevents the raw liquid L from adhering to the stirring blade 44 or the like due to insufficient freezing of the raw liquid L.

[0149] In the particle production apparatus 101 of the second embodiment, the ultrasonic nozzle 31 is attached to the cover portion 12 .

[0150] When the frozen particles A or freeze-dried particles are manufactured using the particle manufacturing device 101 of the second embodiment, the same method as in the first embodiment can be used. In the first embodiment, the frozen particles and the freeze-dried particles are manufactured in separate spaces, respectively, and in the second embodiment, the frozen particles A are manufactured by discharging and freezing the raw material liquid L and the freeze-dried particles are manufactured by stirring and drying the frozen particles A under reduced pressure, which can be performed in the accommodation space 10a of the freezing chamber 10. In the second embodiment, the freezing of the raw material liquid L and the drying of the frozen particles A can be performed in the same space, so it is easy to make the particle manufacturing device 101 smaller than the particle manufacturing device 100 of the first embodiment.

[0151] In the particle manufacturing device 101 of the second embodiment, the raw material liquid L can be discharged from the ultrasonic nozzle 31 while the freezing chamber 10 is maintained at a predetermined vacuum degree, and at the time when a predetermined amount of frozen particles A is obtained, the frozen particles A can be changed to a vacuum degree suitable for drying the frozen particles in a frozen state, and the stirring device 40 can be started to prepare freeze-dried particles. In the second embodiment, it is not always necessary to perform freezing and drying in the freezing chamber 10, for example, the frozen particles A obtained in the freezing chamber 10 can be transferred to another freeze-drying device and dried by the freeze-drying device.

[0152] In this embodiment, freezing and drying can be performed only in the freezing chamber 10, so it is easy to automate. In this embodiment, the movement of the frozen particles is small, so mixing with foreign impurities can be prevented. Therefore, it can be said that this embodiment is suitable for the case where the frozen particles A or the freeze-dried particles are medicines. In the first embodiment, the freezing chamber 10 and the reduced pressure drying chamber 50 are connected by the opening and closing device 60, and in this embodiment, the number of such connections can be reduced, and maintenance work (such as cleaning) can also be simplified.

[0153] (Third embodiment)

[0154] The following will refer to Figure 5 A particle manufacturing apparatus 102 according to a third embodiment is described. In the third embodiment, a drying chamber of a conical dryer is used as the reduced pressure drying chamber 50 of the particle manufacturing apparatus 102. More specifically, the particle manufacturing apparatus 102 of the third embodiment is configured so that the conical dryer is rotated halfway (rotated 180 degrees) to switch from an upright position to a vertical position so that the conical dryer enters an inverted position, and the freezing chamber 10 is connected from above to a product discharge port facing upward.

[0155] The particle manufacturing device 102 of the third embodiment is common to the particle manufacturing device 100 of the first embodiment in that the raw material liquid L is discharged from the ultrasonic nozzle 31 into the accommodating space 10a of the freezing chamber 10 in a reduced pressure state prepared by the reduced pressure device 20 including the vacuum pump 21 to manufacture frozen particles A. That is, in the third embodiment, the discharge port of the conical dryer is used as a supply port for supplying the frozen particles A to the reduced pressure drying chamber 50, and when the drying in the reduced pressure drying chamber 50 is completed, the supply port also serves as the discharge port 51a. In the present embodiment, the freeze-dried particles can be discharged from the reduced pressure drying chamber 50 in a state where the opening direction of the discharge port 51a is downward, and the freeze-dried particles can be discharged by placing the conical dryer in an upright position.

[0156] The freezing chamber 10 of the third embodiment is different from the decompression drying chamber 50 of the first embodiment. The freezing chamber 10 is detachably attached to the decompression drying chamber 50, and a bottom cover 54 is provided in the decompression drying chamber 50 of this embodiment for closing the discharge port 51a after the freezing chamber 10 is detached.

[0157] The particle manufacturing device 102 of the third embodiment is similar to the particle manufacturing device 100 of the first embodiment in that the reduced pressure drying chamber 50 is located below the freezing chamber 10 and is connected to the freezing chamber 10 in the up and down directions, and the reduced pressure drying chamber 50 has a accommodating space 50a capable of receiving the frozen particles A manufactured in the freezing chamber 10.

[0158] The particle manufacturing device 102 of the third embodiment is similar to the particle manufacturing device 100 of the first embodiment in that the reduced pressure drying chamber 50 is connected to the freezing chamber 10 via the opening and closing device 60, and when the opening and closing device 60 is in the open state, the accommodation space 50a is communicated with the accommodation space 10a of the freezing chamber 10. The particle manufacturing device 102 of the third embodiment is similar to the particle manufacturing device 100 of the first embodiment in that the freezing chamber 10 and the reduced pressure drying chamber 50 can be decompressed to a predetermined vacuum degree by the vacuum pump 21 of the decompression device 20.

[0159] The particle manufacturing apparatus 102 of this embodiment is common to the particle manufacturing apparatus 100 of the first embodiment in that the reduced pressure drying chamber 50 includes a main body portion 51 and a cover portion 52, the cover portion 52 is provided with an exhaust port 52a, and the accommodating space 50a is exhausted via a filter unit 53. The particle manufacturing apparatus 102 of the third embodiment is common to the particle manufacturing apparatus 100 of the first embodiment in that a jacket portion 511 through which a heat medium can flow is provided in the reduced pressure drying chamber 50, and the inner wall surface of the reduced pressure drying chamber 50 is a heat transfer surface 50b.

[0160] exist Figure 5 In the particle manufacturing device 102 shown, when the frozen particles A are transferred from the freezing chamber 10, the filter unit 53 is located below. When at least a portion of the filter of the filter unit 53 is exposed to the accommodating space 50a, the frozen particles A may be covered and blocked. Therefore, a covering material that covers the filter unit 53 exposed to the accommodating space 50a from the inside of the chamber can be provided. In order to prevent the adhesion of the frozen particles A, the covering material is preferably made of a material with a higher thermal conductivity than the filter, and is preferably made of a metal (such as stainless steel). The covering material can be made of a porous plate having a mesh larger than the filter of the filter unit 53, and can be formed by a metal mesh or a stamped metal.

[0161] The particle manufacturing device 102 of the third embodiment is different from the particle manufacturing device of the first embodiment in the method of stirring the frozen particles by the stirring device 40. The stirring device 40 in this embodiment includes a pivoting device for pivoting the reduced pressure drying chamber 50, and is configured to stir the frozen particles A contained in the containing space 50a by rotating the reduced pressure drying chamber 50. The stirring device 40 in the particle manufacturing device 102 of the third embodiment includes a rotating mechanism 43, and the stirring device 40 is configured to rotate the reduced pressure drying chamber 50 around the axial center X, which passes through the containing space 50a in the horizontal direction.

[0162] The stirring device 40 of the present embodiment is provided with a swing mechanism (not shown) capable of converting a rotational motion in one direction into a swinging motion, such as a slider crank. The particle manufacturing device 102 of the third embodiment can stir the contained frozen particles A by swinging (pivoting) the reduced pressure drying chamber 50 within a range of +90 degrees to -90 degrees in a state where the reduced pressure drying chamber 50 is connected to the freezing chamber 10 after the frozen particles A are transferred from the freezing chamber 10 to the reduced pressure drying chamber 50, and can also rotate the reduced pressure drying chamber 50 around the axial center X at a predetermined rotation speed in a state where the freezing chamber 10 is removed and the bottom cover 54 is closed. In the latter case, the frozen particles A can be stirred more violently, and the degree of stirring can be adjusted in a wide range. On the other hand, in the latter method, a period of releasing the decompressed state of the primary dry particles is provided until the secondary drying is performed, unless an opening and closing device is provided that is capable of opening and closing the discharge port 51a (the supply port of the primary dry particles) of the decompressed drying chamber 50 in a state connected to the freezing chamber 10, while in the former case, the drying of the frozen particles A can also be performed while maintaining the frozen particles A under the decompressed condition without such a special opening and closing device. If the freezing chamber 10 and the decompressed drying chamber 50 are connected by a flexible pipe, the decompressed drying chamber 50 can be swung while the position of the freezing chamber 10 is fixed.

[0163] In this embodiment, if Figure 5 As shown, the filter unit 53 is located in the inner wall surface of the reduced pressure drying chamber 50 and protrudes in the central direction of the accommodation space 50a. In the present embodiment, when the frozen particles A are produced, the filter unit 53 is located at the bottom portion of the reduced pressure drying chamber 50, so when the amount of the frozen particles A is large, the filter unit 53 may be embedded in the frozen particles A, and the load of the vacuum pump 21 may be increased when the reduced pressure is reduced to form freeze-dried particles. Therefore, when the secondary drying is performed while the reduced pressure drying chamber 50 is swung, it is desirable to adjust the swing angle so that at least a portion of the filter unit 53 is separated from the state of being embedded in the frozen particles A and exposed to the accommodation space 50a.

[0164] In the present embodiment, when the frozen particles A are dried while rotating the reduced pressure drying chamber 50, the frozen particles A contained in the containing space 50a can be completely stirred, and the drying of the frozen particles A can be promoted compared with the first embodiment. The vacuum degree for freezing or drying in the present embodiment can be set to be the same as in the case of the first embodiment. When a conical dryer is used as in the third embodiment, the freezing chamber can also be used as a reduced pressure drying chamber. Such an embodiment will be described below.

[0165] (Fourth embodiment)

[0166] Figure 6A particle production apparatus 103 of a fourth embodiment is shown, and a particle production apparatus 103 using a conical dryer as in the third embodiment is shown. Figure 6 The conical dryer is shown in an upright position. In the third embodiment, the drying chamber of the conical dryer is a reduced pressure drying chamber 50 for performing freeze drying, while in this embodiment, the drying chamber is a freezing chamber 10 for discharging and freezing the raw material liquid L, and the freezing chamber 10 can also dry the frozen particles A under reduced pressure as needed.

[0167] In the particle manufacturing device 103 of the fourth embodiment, the freezing chamber 10 includes a main body portion 11 and a cover portion 12 that closes the upper opening of the main body portion 11. The cover portion 12 is provided with an exhaust port 12a, which is the same as the third embodiment. The freezing chamber 10 has a discharge port 11a in the lower end portion, which can be used as an extraction port for freezing particles A, and a bottom cover 14, which is used to open and close the discharge port 11a.

[0168] The freezing chamber 10 of the fourth embodiment has in common with the reduced pressure drying chamber 50 of the particle manufacturing device 102 of the third embodiment that the filter unit 13 is provided in the exhaust port 12a, and the accommodation space 10a is exhausted through the filter unit 13 by the reduced pressure device 20. The freezing chamber 10 of the fourth embodiment has in common with the reduced pressure drying chamber 50 of the third embodiment that the main body portion 11 has a jacket portion 111, a heat transfer surface 10b for heating or cooling the accommodated object is provided in the main body portion 11, and the temperature of the accommodated frozen particles can be adjusted. The particle manufacturing device 103 of the fourth embodiment has in common with the particle manufacturing device of the third embodiment the configuration or arrangement of the stirring device 40.

[0169] In the particle manufacturing device 103 of the fourth embodiment, the discharge device 30 is fixed to the freezing chamber 10 and can rotate with the freezing chamber 10. In the particle manufacturing device 103, the filter unit 13 can be set at a position farthest from the point where the raw material liquid L is discharged in the form of particles from the ultrasonic nozzle 31, and the frozen particles A can be prevented from passing through the filter unit 13. That is, in the particle manufacturing device 103 of the fourth embodiment, the ultrasonic nozzle 31 and the filter unit 13 can be arranged to be opposite to each other in the freezing chamber 10. In this case, a covering material (filter cover) can be provided so that the filter of the filter unit 13 is not exposed toward the ultrasonic nozzle 31. That is, the covering material can be provided to block the straight line connecting the filter and the ultrasonic nozzle 31. Similar to the filter unit 53 of the third embodiment, the covering material is preferably made of a material having a higher thermal conductivity than the filter, and is preferably made of a metal (such as stainless steel). The covering material can be made of a porous plate having a mesh larger than the filter, and can be formed of a metal mesh or a stamped metal.

[0170] In the particle manufacturing apparatus 103 of the fourth embodiment, an ultrasonic nozzle 31, a pump 32 for supplying a raw material liquid L to the ultrasonic nozzle 31, and a raw material tank 33 for storing the raw material liquid L are fixed to the freezing chamber 10. Figure 6 As shown, one or more ultrasonic nozzles 31 may be provided on one of the left and right walls of the freezing chamber 10 when viewed from a direction orthogonal to the axial center X, which is the pivot center or rotation center of the freezing chamber 10. When the ultrasonic nozzles 31 are arranged in this manner, it is possible to prevent the frozen particles A contained in the freezing chamber 10 from covering the discharge port 31a of the ultrasonic nozzle 31 even when the frozen particles A are stirred by rotating the freezing chamber 10 while discharging the raw material liquid L, and it is also possible to prevent the discharge port 31a from being clogged, and to reduce the formation of agglomerates in which a plurality of frozen particles A are agglomerated by the discharged raw material liquid.

[0171] When the frozen particles A or freeze-dried particles are manufactured using the particle manufacturing device 103 of the fourth embodiment, the same method as in the first embodiment can be used. In the first embodiment, the formation of the frozen particles A and the formation of the freeze-dried particles are respectively performed in the freezing chamber 10 and the reduced pressure drying chamber 50, which are separate chambers, and in the fourth embodiment, as in the second embodiment, the formation of the frozen particles A and the formation of the freeze-dried particles are performed in a single chamber used as both the freezing chamber 10 and the reduced pressure drying chamber 50. In the fourth embodiment, the formation of the frozen particles A and the formation of the freeze-dried particles can be performed in the same space, and the particle manufacturing device 103 can be easily miniaturized.

[0172] In the particle manufacturing device 103 of the fourth embodiment, the raw material liquid L can be discharged from the ultrasonic nozzle 31 while the freezing chamber 10 is maintained at a predetermined vacuum degree, and the frozen particles A can be changed to a vacuum degree suitable for drying the frozen particles A to prepare freeze-dried particles at a time when a predetermined amount of frozen particles A is obtained. The stirring device 40 may be driven both when the frozen particles A are formed by discharging the raw material liquid L and when the frozen particles A are dried by increasing the vacuum degree, may be driven in only one of the two cases, or may not be driven in either case.

[0173] For example, when the stirring device 40 is used for both freezing and freeze-drying, the freezing chamber 10 may be swung only during freezing, and the freezing chamber 10 may be rotated during freeze-drying.

[0174] In the particle manufacturing device 103 of the fourth embodiment, the attachment position of the ultrasonic nozzle 31 is shown to be significantly changed relative to the attachment position of the third embodiment, and the attachment position of the ultrasonic nozzle 31 in the fourth embodiment can be the discharge port 11a as in the third embodiment.

[0175] In the present embodiment, the discharge device 30 may be separated between the ultrasonic nozzle 31 attached to the freezing chamber 10 and the device upstream of the ultrasonic nozzle 31 (for example, between the ultrasonic nozzle 31 and the pump 32), the raw material tank 33 or the pump 32 may be removed, and the frozen particles A may be dried by rotating the freezing chamber 10 while leaving only the ultrasonic nozzle 31 attached to the freezing chamber 10. In this case, after the frozen particles A are formed, the decompression state of the freezing chamber 10 may be prevented from being released by drying the frozen particles A while the ultrasonic nozzle 31 is attached.

[0176] After the ultrasonic nozzle 31 is removed from the freezing chamber 10 , the frozen particles A may be dried. In this case, the frozen particles A do not cover the ultrasonic nozzle 31 during the rotation of the freezing chamber 10 , so clogging of the discharge port 31 a of the ultrasonic nozzle 31 may be more reliably prevented.

[0177] In the fourth embodiment or the second embodiment, as in the first embodiment or the third embodiment, the freezing chamber for freezing the raw material liquid L and the reduced pressure drying chamber for drying the frozen particles A may not be prepared separately, so the device can be made compact. In addition, in the second embodiment or the fourth embodiment, a wide accommodation space can be ensured for discharging the raw material liquid from the ultrasonic nozzle, so it is easy to prevent the frozen raw material liquid from becoming an adherent substance and adhering to the inner wall of the freezing chamber, etc.

[0178] In the second embodiment or the fourth embodiment, even if adhered matter is generated on the wall surface of the freezing chamber, etc., the adhered matter is caused to fall off by the stirring device that stirs the frozen particles. In particular, in the fourth embodiment, when the frozen particles A are dried, the freezing chamber itself can be rotated, thereby making it easy to separate the adhered matter. In the particle manufacturing device or the method for manufacturing frozen particles in the fourth embodiment, various modifications can be made without being limited to the above examples as in the above embodiments.

[0179] The frozen particles A manufactured in this embodiment may be particles (primary particles) in a state of being discharged from the ultrasonic nozzle in the form of particles, or may be particles in which some or all of the particles discharged from the ultrasonic nozzle are bonded to each other (agglomerated particles). The particle manufacturing device of this embodiment can be used not only to prepare frozen particles or freeze-dried particles, but also to perform secondary processing. For example, the particle manufacturing device of this embodiment can be used to crush freeze-dried particles to form refined particles, cover frozen particles or freeze-dried particles with a coating agent to form core-shell particles, or attach frozen particles or freeze-dried particles to other particles to form composite particles.

[0180] As described above, in this embodiment, frozen particles can be formed quickly while preventing nozzle clogging, and frozen particles can be easily prepared. The present invention is not limited to the above embodiment, and various modifications can be made. That is, the present invention is not limited to the above example.

[0181] As described above, the present invention includes the following disclosures.

[0182] A particle manufacturing device includes: a freezing chamber, which is configured to accommodate frozen particles, and the frozen particles are obtained by freezing an object to be processed in the form of particles containing water; an ultrasonic nozzle, which is configured to discharge the object to be processed in the form of particles after or before freezing into the freezing chamber; and a decompression device, which is configured to decompress the freezing chamber, wherein the water evaporates due to the decompression, and the frozen particles are cooled and frozen by the evaporation of the water.

[0183] The particle manufacturing device of the present invention has the above configuration, so that frozen particles can be quickly manufactured while preventing the clogging of the nozzle due to freezing. According to one aspect of the present invention, when the frozen particles are manufactured, the pressure in the freezing chamber is stable, and frozen particles with uniform size can be formed. In addition, according to another aspect of the present invention, the delivery power required for discharging the object to be processed from the ultrasonic nozzle can be reduced.

[0184] The particle manufacturing device may include a reduced pressure drying chamber for drying the frozen particles under reduced pressure to form freeze-dried particles, the reduced pressure drying chamber also serving as a freezing chamber or being a chamber separate from the freezing chamber, and may also include a stirring device for stirring the frozen particles, and the stirring device may be configured to stir the frozen particles in the freezing chamber or the reduced pressure drying chamber. According to such a preferred aspect, freeze-dried particles can be efficiently prepared using frozen particles.

[0185] The particle manufacturing device is configured so that the stirring device includes a pivot device, and the pivot device pivots the freezing chamber, and the frozen particles contained in the freezing chamber can be stirred by the pivoting of the freezing chamber, and the freezing chamber can also be used as the reduced pressure drying chamber, so that the frozen particles can be stirred while forming the frozen particles, and the frozen particles can be dried while stirring the frozen particles. According to such a preferred aspect, not only can space saving be achieved, but also freeze-dried particles can be effectively prepared using frozen particles. In addition, according to such a preferred aspect, space can be saved, so it can also be ensured that there is a wider space for the freezing chamber, and the discharged raw material liquid can be prevented from adhering to the inside of the freezing chamber.

[0186] The particle manufacturing device may include a reduced pressure drying chamber, which is a chamber separated from the freezing chamber, and the stirring device may include a pivoting device, which pivots the reduced pressure drying chamber, and the frozen particles contained in the reduced pressure drying chamber can be stirred by the pivoting of the reduced pressure drying chamber. According to such a preferred aspect, the freezing chamber and the reduced pressure drying chamber have different configurations, thereby widening the application range of the process. For example, in this preferred aspect, the following process can also be adopted, that is, while the frozen particles prepared in the freezing chamber are transferred to the reduced pressure drying chamber and dried in the reduced pressure drying chamber, the next frozen particles are prepared in the freezing chamber.

[0187] The particle manufacturing device is configured so that the stirring device includes a rotating body, the rotating body rotates in the freezing chamber around the axial center passing through the freezing chamber, and the frozen particles contained in the freezing chamber can be stirred by the rotation of the rotating body, and the freezing chamber can also be used as the reduced pressure drying chamber, so that the frozen particles can be stirred while forming the frozen particles, and the frozen particles can be dried while stirring the frozen particles. According to such a preferred aspect, not only can space saving be achieved, but also freeze-dried particles can be effectively prepared using frozen particles. In addition, according to such a preferred aspect, space can be saved, so it is also possible to ensure that there is a wider space for the freezing chamber, and the discharged raw material liquid can be prevented from adhering to the inside of the freezing chamber.

[0188] The particle manufacturing device may include a reduced pressure drying chamber, which is a chamber separated from the freezing chamber, and the stirring device may include a rotating body, which rotates in the reduced pressure drying chamber around an axial center passing through the reduced pressure drying chamber, and the frozen particles contained in the reduced pressure drying chamber can be stirred by the rotation of the rotating body. According to such a preferred aspect, not only space saving can be achieved, but also freeze-dried particles can be effectively prepared using frozen particles. In addition, according to such a preferred aspect, space can be saved, so a wider space can be ensured for the freezing chamber, and the injected and discharged raw material liquid can be prevented from adhering to the inside of the freezing chamber.

[0189] The particle manufacturing device further includes: a temperature regulating device, the temperature regulating device being configured to heat or cool the object to be processed to be discharged from the ultrasonic nozzle when the object to be processed passes through the ultrasonic nozzle. According to such a preferred aspect, blockage due to freezing can be further prevented.

[0190] In the particle manufacturing device, the object to be processed may also contain an organic solvent whose freezing point and boiling point are lower than those of water. According to such a preferred aspect, agglomeration of frozen particles can be reduced, and frozen particles with uniform size can be stably prepared.

[0191] In the particle manufacturing device, the freezing chamber may be provided with an exhaust port, the exhaust port being used to evacuate the freezing chamber so that the interior of the freezing chamber is in a decompressed state, and the ultrasonic nozzle and the exhaust port may be arranged at an upper portion of the freezing chamber. According to this aspect, the frozen particles can be prevented from being discharged to the outside of the device in an unexpected form.

[0192] In the particle production device, the ultrasonic nozzle and the exhaust port may be arranged away from each other at positions opposite to each other with respect to the center of the freezing chamber. According to this aspect, the frozen particles can be further prevented from being discharged to the outside of the device in an unintended form.

[0193] A method for producing frozen particles, wherein the frozen particles are obtained by freezing an object to be processed in the form of particles by the following steps: a step of decompressing the object to be processed containing moisture and cooling and freezing the object to be processed by evaporating the moisture; and a step of forming the frozen object to be processed or the unfrozen object to be processed in the form of particles by an ultrasonic nozzle.

[0194] According to the present invention, frozen particles can be efficiently prepared.

[0195] The method for producing frozen particles can also perform a drying step of drying the frozen particles under a reduced pressure environment, and in the drying step, the frozen particles can be stirred in a reduced pressure space. According to such a preferred aspect, not only frozen particles can be efficiently prepared, but also freeze-dried particles can be efficiently produced.

[0196] The object to be processed may further contain an organic solvent having a freezing point and a boiling point lower than those of water. According to the manufacturing method in such a preferred aspect, agglomeration of frozen particles can be reduced, and frozen particles or freeze-dried particles having uniform sizes can be stably prepared.

[0197] As described above, according to the present disclosure, a particle manufacturing apparatus and a method for manufacturing frozen particles that can quickly manufacture frozen particles while reducing nozzle clogging due to freezing can be provided.

[0198] Reference numerals list

[0199] 10: Freezing Chamber

[0200] 20: Pressure relief device

[0201] 30: Discharge device

[0202] 31: Ultrasonic nozzle

[0203] 40: Stirring device

[0204] 44: Mixing blade

[0205] 50: Decompression drying chamber

[0206] 100, 101, 102, 103: Particle manufacturing device

Claims

1. A particle manufacturing device, comprising: a freezing chamber configured to accommodate frozen particles obtained by freezing an object to be processed in the form of particles containing moisture; a decompression device configured to decompress the freezing chamber, and an ultrasonic nozzle configured to discharge the object to be processed in the form of particles into the freezing chamber depressurized by the depressurizing device, wherein The frozen particles are produced due to freezing of the object to be processed by cooling caused by evaporation of water from the object to be processed under a reduced pressure environment.

2. The particle production device according to claim 1, in, The freezing chamber is used to dry the frozen particles under reduced pressure to form freeze-dried particles, and The particle manufacturing device further includes a stirring device configured to stir the frozen particles in the freezing chamber.

3. The particle manufacturing device according to claim 1, comprising: Freezing chamber; a reduced pressure drying chamber configured to dry the frozen particles obtained in the freezing chamber under a reduced pressure environment to form freeze-dried particles; and A stirring device is configured to stir the frozen particles in the reduced pressure drying chamber.

4. The particle production device according to claim 2, wherein: The stirring device comprises a pivoting device configured to pivot the freezing chamber such that the frozen particles contained in the freezing chamber are stirred by pivoting the freezing chamber.

5. The particle production device according to claim 3, wherein: The stirring device includes a pivot device configured to pivot the reduced-pressure drying chamber so that the frozen particles contained in the reduced-pressure drying chamber are stirred by pivoting the reduced-pressure drying chamber.

6. The particle production device according to claim 2, wherein: The stirring device includes a rotating body that rotates in the freezing chamber about an axial center passing through the freezing chamber so that frozen particles contained in the freezing chamber are stirred by the rotation of the rotating body.

7. The particle production device according to claim 3, wherein: The stirring device includes a rotating body that rotates in the reduced-pressure drying chamber about an axial center passing through the reduced-pressure drying chamber, so that frozen particles contained in the reduced-pressure drying chamber are stirred by rotation of the rotating body.

8. The particle manufacturing device according to any one of claims 1 to 7, further comprising: A temperature regulating device is configured to heat or cool the object to be processed to be discharged from the ultrasonic nozzle when the object to be processed passes through the ultrasonic nozzle.

9. The particle production device according to any one of claims 1 to 8, wherein: The object to be processed further contains an organic solvent, and The freezing point and boiling point of the organic solvent are lower than the freezing point and boiling point of water.

10. The particle production device according to claim 1, wherein: The freezing chamber is provided with an exhaust port, and the exhaust port is used to evacuate the freezing chamber so that the interior of the freezing chamber is in a decompressed state, and The ultrasonic nozzle and the exhaust port are arranged at an upper portion of the freezing chamber.

11. The particle production device according to claim 10, wherein: The ultrasonic nozzle and the exhaust port are arranged at positions opposing each other with respect to the center of the freezing chamber.

12. A method for producing frozen particles, comprising: The object to be processed containing moisture is formed into a granular form by an ultrasonic nozzle; as well as before the object to be processed is formed into a particle form by the ultrasonic nozzle, or after the object to be processed is formed into a particle form by the ultrasonic nozzle, freezing the object to be processed to produce frozen particles, wherein the object to be processed is frozen in the particle form, The freezing of the object to be processed is achieved by cooling the object to be processed, and the cooling is caused by evaporation of water.

13. The method for producing frozen particles according to claim 12, further comprising: Drying the frozen particles under reduced pressure, Wherein, during the drying, the frozen particles are stirred in a reduced pressure space.

14. The method for producing frozen particles according to claim 12 or 13, wherein: The object to be processed further contains an organic solvent, and the freezing point and boiling point of the organic solvent are lower than those of water.

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