Powder removal device for vacuum spray freeze drying apparatus, powder removal method for vacuum spray freeze drying apparatus, and vacuum spray freeze drying apparatus

Abstract

To provide a powder extraction device in a vacuum spray freeze drying device, to be used for a vacuum spray freeze drying device, capable of easily extracting a small amount of test powder stored in a container with the performance and characteristics equivalent to those of a product mass-produced in a continuous vacuum freeze spray drying device, with a small amount of a raw material.SOLUTION: A powder extraction device 100 in a vacuum spray freeze drying device, comprises a drying unit 10 connected to a frozen fine particle forming unit spraying liquid droplets into vacuum to form frozen fine particles, and a recovery unit 20 connected to the drying unit 10, with the drying unit 10 and the recovery unit 20 forming a decompression space together with the frozen fine particle forming unit 40, the drying unit 10 comprising a receiving table 11 receiving the frozen fine particles formed in the frozen fine particle forming unit 40, to form powder by drying the frozen fine particles in a state of being placed on the receiving table 11. The recovery unit 20 recovers the powder placed on the receiving table 11 into a container 30 and seals the container 30.SELECTED DRAWING: Figure 1

Description

[Technical field]

[0001] The present invention relates to a powder removal device for a vacuum spray freeze drying apparatus, a powder removal method for a vacuum spray freeze drying apparatus, and a vacuum spray freeze drying apparatus. More specifically, the present invention relates to a powder removal device for a vacuum spray freeze drying apparatus, a powder removal method for a vacuum spray freeze drying apparatus, and a vacuum spray freeze drying apparatus, which are devices used for a vacuum spray freeze drying apparatus and can efficiently and easily produce a small amount of containerized test powder having the same performance and properties as products mass-produced by a continuous vacuum freeze drying apparatus and remove the powder from the container in a simple manner. [Background technology]

[0002] Conventionally, in the manufacturing process of medicines, foods, cosmetics, etc., a vacuum spray freeze drying apparatus is used to spray the raw material liquid of medicines, foods, cosmetics, etc. into a vacuum to obtain powdered medicines, foods, cosmetics, etc. The raw material liquid is a solution or dispersion of the raw materials of medicines, foods, cosmetics, etc. in a solvent or dispersion medium, and this raw material liquid is sprayed into the vacuum space in the vacuum spray freeze drying apparatus to become frozen fine particles. The frozen fine particles are then sublimated and dried to obtain a powder.

[0003] Various types of vacuum spray freeze drying apparatus have been reported, including an apparatus that includes a vacuum chamber into which the raw material liquid is sprayed and a shelf that receives the frozen raw material, and that dries the frozen particles on the shelf after receiving them on the shelf (see, for example, Patent Document 1), and an apparatus that is used in the manufacture of pharmaceuticals and can perform vacuum freeze drying continuously in a short period of time (see, for example, Patent Document 2).The vacuum drying apparatus in Patent Document 2 is a continuous vacuum drying apparatus that is different from a batch type apparatus in that powders such as pharmaceuticals are continuously and sequentially manufactured while raw materials are being supplied.

[0004] The powdered medicines and the like thus produced are then filled into containers such as vials and sealed (see, for example, Patent Document 3), and when required, they can be redissolved or used in their original powdered form. [Prior art documents] [Patent documents]

[0005] [Patent Document 1] International Publication No. 2010 / 005021 [Patent Document 2] Patent No. 6777350 [Patent Document 3] Utility Model Registration No. 3117063 Summary of the Invention [Problem to be solved by the invention]

[0006] Here, in the testing and development stages of new products, it is necessary to conduct evaluation tests on preservation stability, efficacy, etc. before distributing them on the market. In other words, it is necessary to confirm and evaluate the efficacy after freeze-drying, the properties after a certain period of storage, and resolubility.

[0007] In this case, a small amount of sample is sufficient for the evaluation test. However, for example, a vacuum freeze-drying device (vacuum spray freeze-drying device) capable of continuously performing vacuum freeze-drying as described in Patent Document 2 can perform the vacuum freeze-drying process in a short time as described above, and is useful for manufacturing actual products (mass production). However, because the drying process is performed in a cylindrical section, it is necessary to prepare a relatively large amount of raw material to obtain a powder. In other words, although a small amount of sample is sufficient for the evaluation test, when the vacuum freeze-drying device described in Patent Document 2 is used to obtain this sample, a relatively large amount of raw material is required as described above, and there is a lot of waste of raw material.

[0008] Therefore, while it is assumed that the continuous vacuum freeze-drying apparatus of Patent Document 2 will be used for mass production, when preparing samples for evaluation tests, it is important to appropriately produce only the amount required for the evaluation tests, and it is also important to avoid wasting raw materials. In particular, in the case of pharmaceuticals, the raw materials are often valuable and expensive, and there is a strong demand for such materials, so it is desirable to be able to produce the required amount of powder for evaluation tests without wasting raw materials as much as possible (i.e., with high production efficiency).

[0009] For these reasons, it was necessary to develop a vacuum spray freeze drying apparatus capable of producing small amounts of powder for evaluation tests to evaluate the performance and properties of products produced by the continuous vacuum freeze drying apparatus (especially products made from rare and expensive raw materials such as pharmaceuticals), a powder removal device for this vacuum spray freeze drying apparatus, and a method for removing powder from the vacuum spray freeze drying apparatus.

[0010] The present invention has been made to solve the problems of the prior art as described above, and provides a vacuum spray freeze drying apparatus that can efficiently and easily produce small amounts of containerized test powder having performance and properties equivalent to those of products mass-produced by a continuous vacuum freeze drying apparatus, a powder removal device for this vacuum spray freeze drying apparatus, and a method for removing powder from the vacuum spray freeze drying apparatus. [Means for solving the problem]

[0011] According to the present invention, there are provided the following powder removal device for a vacuum spray freeze drying apparatus, a powder removal method for a vacuum spray freeze drying apparatus, and a vacuum spray freeze drying apparatus.

[0012] [1] Droplets in a vacuum 1~100ml / min Being sprayed Particle size 30~300μm a drying section connected to the frozen particle forming section for forming frozen particles; A recovery section connected to the drying section, The drying section and the recovery section form a single reduced pressure space together with the frozen particle forming section, the drying unit has a receiving stand for receiving the frozen particles formed in the frozen particle forming unit, and dries the frozen particles in a state in which the frozen particles are placed on the receiving stand to form a powder body; The recovery section includes: A container is placed inside, The powder on the receiving table The 1. A powder removal device for a vacuum spray freeze drying apparatus, which recovers powder in a container and seals the container.

[0013] [2] The collection unit has a moving unit that moves the container within the collection unit, The collecting section has a lid holder at its upper portion for holding a lid for sealing the container, and a lifting section for moving the container up and down to seal the container with the lid. A powder removal device for the vacuum spray freeze drying apparatus described in [1] above.

[0014] [3] The powder removal device in the vacuum spray freeze drying apparatus described in [2], wherein the moving part is provided with a fixing part for fixing the container.

[0015] [4] The powder removal device in the vacuum spray freeze drying apparatus according to any one of the above [1] to [3], which is part of a continuous vacuum spray freeze drying apparatus for producing powder for pharmaceutical testing.

[0016] [5] The above-mentioned [1] further comprises a gas supply unit for supplying an inert gas or dehumidified air into the reduced pressure space. ~[3] 2. A powder removal device for the vacuum spray freeze drying apparatus according to claim 1 .

[0017] [6] The powder removal device for the vacuum spray freeze drying apparatus described in [5] above, wherein the inert gas or dehumidified air is a sterilized gas and is supplied so as to set the pressure in the reduced pressure space to 10 to 80 kPa.

[0018] [7] The container is a sterilized container, ~[3] 2. A powder removal device for the vacuum spray freeze drying apparatus according to claim 1 .

[0019] [8] See above[1] ~[3] A method for extracting powder in a vacuum spray freeze drying apparatus using the powder extracting device in the vacuum spray freeze drying apparatus described in A method for extracting powder in a vacuum spray freeze drying apparatus, comprising drying the frozen fine particles formed by the frozen fine particle formation section on the receiving stand of the drying section, then pouring the dried powder from the receiving stand into the container arranged in the recovery section, and sealing the container into which the powder has been poured.

[0020] [9] The method for extracting powder in a vacuum spray freeze drying apparatus described in [8], wherein the receiving table rotates so that the surface on which the frozen fine particles are placed is inclined.

[0021]

[10] After the powder is added to the container, Inert gas or dehumidified air is supplied into the reduced pressure space. The method for extracting powder in a vacuum spray freeze drying apparatus described in [8] above, further comprising: supplying an inert gas or dehumidified air into the reduced pressure space by a gas supply unit; and then sealing the container.

[0022]

[11] The method for extracting powder in the vacuum spray freeze drying apparatus described in

[10] above, wherein a sterilized gas is used as the inert gas or dehumidified air, and the gas is supplied so that the pressure in the reduced pressure space is 10 to 80 kPa.

[0023]

[12] The container is a sterilized container. ] A method for removing powder from the vacuum spray freeze drying apparatus described above.

[0024]

[13] A frozen particle forming section in which droplets are sprayed into a vacuum to form frozen particles; [1] ~[3] 13. A vacuum spray freeze drying apparatus comprising: a powder removal device for the vacuum spray freeze drying apparatus described in claim 12.

[0025]

[14] The droplets are 30 The vacuum spray freeze drying apparatus according to

[13] , wherein the spray rate is 1 ml / min. Effect of the Invention

[0026] The powder removal device in the vacuum spray freeze drying apparatus of the present invention is an apparatus used as part of a vacuum spray freeze drying apparatus for producing test powders for pharmaceuticals, etc., and has the effect of enabling the efficient and easy production of small amounts of containerized test powder having performance and properties equivalent to those of products mass-produced by a continuous vacuum freeze drying apparatus, from which the powder can be removed.

[0027] According to the powder extraction method in the vacuum spray freeze drying apparatus of the present invention, it is possible to efficiently and easily produce small amounts of containerized test powder having performance and properties equivalent to those of products mass-produced in a continuous vacuum freeze drying apparatus, by using a vacuum spray freeze drying apparatus equipped with the extraction device of the present invention.

[0028] The vacuum spray freeze drying apparatus of the present invention has the effect of enabling efficient and simple production of small amounts of containerized test powder having performance and properties equivalent to those of products mass-produced by a continuous vacuum freeze drying apparatus. [Brief description of the drawings]

[0029] [Figure 1] FIG. 1 is a schematic side view showing, in perspective, a portion of one embodiment of a vacuum spray freeze drying apparatus according to the present invention. [Diagram 2] FIG. 2 is an explanatory diagram showing a schematic diagram of one embodiment of a powder removal method in the vacuum spray freeze drying apparatus of the present invention. [Diagram 3] FIG. 2 is an explanatory diagram showing a schematic diagram of one embodiment of a powder removal method in the vacuum spray freeze drying apparatus of the present invention. [Figure 4] FIG. 2 is an explanatory diagram showing a schematic diagram of one embodiment of a powder removal method in the vacuum spray freeze drying apparatus of the present invention. [Diagram 5] FIG. 2 is an explanatory diagram showing a schematic diagram of one embodiment of a powder removal method in the vacuum spray freeze drying apparatus of the present invention. [Figure 6] FIG. 2 is an explanatory diagram showing a schematic diagram of one embodiment of a powder removal method in the vacuum spray freeze drying apparatus of the present invention. [Figure 7]FIG. 2 is an explanatory diagram showing a schematic diagram of one embodiment of a powder removal method in the vacuum spray freeze drying apparatus of the present invention. [Figure 8] FIG. 3 is a side view corresponding to FIG. 2 and typically showing another embodiment of the vacuum spray freeze drying apparatus of the present invention. [Figure 9] FIG. 3 is a side view corresponding to FIG. 2 and typically showing a vacuum spray freeze drying apparatus according to still another embodiment of the present invention. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS

[0030] The following describes the embodiments of the present invention, but the present invention is not limited to the following embodiments. In other words, it should be understood that the scope of the present invention includes any modifications and improvements to the following embodiments based on the ordinary knowledge of a person skilled in the art without departing from the spirit of the present invention.

[0031] (1) Powder removal device for vacuum spray freeze drying equipment: One embodiment of the powder extracting device in the vacuum spray freeze drying apparatus of the present invention is a powder extracting device 100 in the vacuum spray freeze drying apparatus 200 shown in Fig. 1. This extracting device 100 is a device for extracting powder in which droplets are immersed in a vacuum. 1~100ml / min Being sprayed Particle size 30~300μm The apparatus is provided with a drying section 10 connected to a frozen particle forming section 40 which forms frozen particles, and a collection section 20 connected to the drying section 10. When producing a powder, the drying section 10 and the collection section 20 form a single reduced pressure space together with the frozen particle forming section 40. The drying section 10 has a receiving table 11 which receives the frozen particles formed in the frozen particle forming section 40, and dries the frozen particles while they are placed on the receiving table 11 to form a powder. The collection section 20 has A container 30 is disposed therein, The powder on the receiving stand 11 is collected in a container 30, and then the container 30 is sealed.

[0032] The "reduced pressure space" means a space with a pressure lower than atmospheric pressure, and includes a vacuum space. The vacuum is the same as the vacuum in a conventionally known vacuum freeze-drying device. Specifically, it can be said to be a pressure state of about 0.7 kPa or less.

[0033] This take-out device 100 is used as part of a vacuum spray freeze-drying device for producing test powders, such as pharmaceuticals, whose raw materials are valuable or expensive, and can produce a small amount of containerized test powder having the same performance and properties as products mass-produced by a continuous vacuum freeze-drying device, and can easily take it out efficiently (i.e., with little waste of raw materials). Since this test powder has the same performance and properties as products mass-produced by a continuous vacuum freeze-drying device, the properties of the powder (e.g., effect expression, storage stability) can be evaluated before the product is distributed to the market.

[0034] The drying section 10 and the collection section 20 form a single reduced pressure space together with the frozen particle formation section 40. That is, the droplets sprayed into the frozen particle formation section 40 become frozen particles in a vacuum atmosphere, are dried in the drying section 10 in a vacuum atmosphere to become a powder, and the powder is collected in the container 30 arranged in the collection section 20, and the container 30 is sealed. After sealing the container 30 in this manner, the vacuum atmosphere can be released and the pressure can be returned to normal, and the container 30 can be collected.

[0035] Since the raw materials of the test powder are valuable or expensive, the amount of the raw material liquid sprayed (amount of sprayed droplets) is small. Specifically, the droplets can be sprayed at 1 to 100 ml / min, preferably 1 to 30 ml / min, and more preferably 2 to 10 ml / min.

[0036] The powder under test is not limited to pharmaceuticals; it can also be cosmetics or food. However, since pharmaceuticals are often made from rare and expensive raw materials, the use of the device of the present invention is highly effective.

[0037] Furthermore, there is no particular restriction on the particle size of the frozen fine particles, but in the case of pharmaceuticals, for example, the particle size can be about 30 to 300 μm.

[0038] (1-1)Drying section: As shown in FIG. 1, the drying section 10 has a receiving table 11 that receives the frozen particles formed in the frozen particle forming section 40, and dries the frozen particles while they are placed on the receiving table 11 to form a powder.

[0039] The time for drying the frozen particles on the receiving table 11 can be set according to the manufacturing conditions of the powder to be tested. When the spraying of the raw material is finished and the drying of the frozen particles is started, the pressure in the drying section 10 is further reduced. When the pressure in the drying section 10 is completely reduced, the drying of the frozen particles is completed.

[0040] That is, for example, in the vacuum freeze-drying apparatus described in Patent Document 2, frozen particles are supplied to a horizontally long drying device (cylindrical part) for drying, but a certain amount of frozen particles is required to supply the frozen particles to this drying device. On the other hand, when the purpose is to evaluate and test the properties of a powder, a large amount of powder is not necessary, and especially when the powder is valuable or expensive, such as a raw material for medicines, producing such a large amount of powder is wasteful in terms of raw material procurement and costs. Therefore, by providing a drying section 10 as in the present invention and drying, a small amount of test powder can be produced efficiently and easily.

[0041] It is preferable that the lower portion of the drying section 10 is narrowed, and the opening of the outlet portion of the drying section 10 is approximately the same size as the mouth of the container 30. In this way, the powder can be easily collected from the drying section 10 to the container 30.

[0042] (1-1a) Receiving stand: There are no particular limitations on the shape or size of the receiving table 11, so long as it can receive the frozen particles dropping from the frozen particle forming section 40 and can hold the received frozen particles for a predetermined period of time.

[0043] For example, a single flat plate can be used as the receiving stand 11. The flat receiving stand 11 may be one that can be divided in the center. When the flat plate is one that can be divided in the center, the powder can be moved to the collecting section 20 by dividing the flat plate.

[0044] The receiving table 11 can be rotated so that the surface on which the frozen particles are placed is inclined. By inclining the receiving table 11 in this manner, the powder can be easily transferred from the receiving table 11 to the recovery section 20.

[0045] There is no particular restriction on the material of this receiving table 11, but if the surface on which the frozen particles are placed is made of stainless steel or Teflon (registered trademark), the drying process of the frozen particles is carried out satisfactorily.

[0046] In addition, a coating may be formed on the surface of the receiving table 11 on which the frozen particles are placed so that the dried frozen particles (powder) can easily move to the collection section 20.

[0047] The receiving stand 11 may be capable of being vibrated. In this case, the receiving stand 11 may be capable of being vibrated manually, or a vibrating unit for vibrating the receiving stand 11 may be provided. This vibrating unit may be a conventionally known vibrating means such as an ultrasonic vibrator. If the receiving stand 11 can be vibrated in this manner, even if the dried frozen fine particles (powder) adhere to the receiving stand 11 and are difficult to move, the dried frozen fine particles (powder) can be easily moved to the collection unit 20.

[0048] (1-2) Recovery section: The collecting unit 20 collects the powder on the receiving table 11 into the container 30, and then seals the container 30. The collecting unit 20 allows the powder to be collected into the container 30 while maintaining a reduced pressure space such as a vacuum atmosphere. Some medicines may deteriorate due to oxidation when stored in the presence of oxygen, so sealing under vacuum conditions, for example, improves the shelf life. Note that some types of medicines tolerate the coexistence of dehumidified oxygen, so an appropriate storage gas may be selected.

[0049] The container 30 is not particularly limited and can be any suitable container as long as it can be sealed. Conventionally known containers can be used, such as vials (see FIG. 1).

[0050] In particular, when the evaluation test subject is a pharmaceutical product that requires high sterility, it is preferable to use a sterilized container 30. Conventionally known conditions can be used as the sterilization conditions.

[0051] There is no particular limit to the number or size of the containers 30, and one to five may be arranged, with one or two being preferred. Figs. 8 and 9 each show an example in which two containers 30 are arranged in a row, and a tall, wide-mouthed container (vial) 130 is arranged. Fig. 9 also shows an example in which 130 is used. As shown in Fig. 9, in an embodiment without the second lifting section 29, it is preferred that the container has a wide mouth (for example, about 13 mm). In this case, the outlet of the drying section 10 (the spout for pouring into the wide-mouthed container) can have an inner diameter of about 10 mm.

[0052] The container 30 can be sealed with a lid 31. Any conventionally known lid can be used as the lid 31, and examples of the lid include a lid made of rubber. When a sterilized container is used, it is preferable to use a sterilized lid 31 as well.

[0053] (1-2a) Moving part: The collection unit 20 may have a moving unit 21 that moves the container 30 within the collection unit 20. There are no particular limitations on the moving unit 21 as long as it can move the container 30 placed within the collection unit 20 from outside the collection unit 20. For example, as shown in Fig. 1, the moving unit 21 may include a fixing unit 23 that fixes the container 30, and a rod-shaped member 25 that is connected to the fixing unit 23 and extends left and right. The container 30 can be moved to a desired position by pushing and pulling the rod-shaped member 25 left and right.

[0054] (1-2b) Lid holding part: The collection unit 20 can have a lid body holding part on the inner surface side of the upper part thereof, which holds the lid body 31 that seals the container 30. By having the lid body holding part, the mouth of the container 30 is pressed against the lid body 31, and then the container 30 is pulled down, whereby the lid body 31 is released from the lid body holding part, and the container 30 is easily sealed.

[0055] (1-2c) Lifting section: The collection unit 20 can have a lifting unit 27 that moves the container 30 up and down in order to plug the container 30 with the lid 31. By providing this lifting unit 27, the lid 31 can be pressed against the mouth of the container 30, thereby fitting the lid 31 to the mouth of the container 30.

[0056] The lifting section 27 may have a support 27a that supports the container 30 from below, and a movement restricting section 27b that stops the movement of the support 27a. Examples of the movement restricting section 27b include a stopper and a spring. Since the inside of the collection section 20 is in a vacuum state, if the movement restricting section 27b that is a member that stops the movement of the support 27a is not provided, the support 27a will push the container 30 upward. Therefore, the movement restricting section 27b restricts unintended movement of the support 27a.

[0057] Here, when two containers 30, 130 are arranged in a row as shown in Figs. 8 and 9, two lifting sections 27 can also be arranged in a row.

[0058] As shown in Fig. 1 and Fig. 8, the recovery section 20 may further include a second lifting section 29 disposed below the inlet through which the powder is fed from the drying section 10 into the container 30. As shown in Fig. 9, the recovery section 20 may be configured without the second lifting section 29. In this case, the device can be simplified.

[0059] The second lifting section 29 is located below the inlet through which the powder is introduced into the container 30, and can lift the container 30 so as to bring the container 30 closer to the inlet. By providing such a second lifting section 29, containers 30 of different heights can be used. That is, containers of different heights may be used as necessary. In that case, the distance between the inlet and the container 30 may differ, but even if the distance between the inlet and the container 30 differs, the height position of the container can be appropriately adjusted by providing the second lifting section 29. In addition, when the second lifting section 29 is provided, the second lifting section 29 can have a support 29a that supports the container 30 from below and a movement restricting section 29b that stops the movement of the support 29a.

[0060] (1-2d) Other structures: The collecting section 20 is preferably provided with an observation window so that the position of the container 30 and the like can be seen from the side of the collecting section 20.

[0061] (1-3) Gas supply unit: The powder extracting device in the vacuum spray freeze drying apparatus of the present invention may further include a gas supplying section for supplying an inert gas or dehumidified air into the reduced pressure space. By providing this gas supplying section, after the powder is collected in the container 30, an inert gas or dehumidified air can be supplied into the container 30.

[0062] In other words, if the container 30 is sealed with the lid 31 while maintaining the vacuum atmosphere after collecting the powder in the container 30, the inside of the container 30 is in a vacuum state, so that when the reduced pressure (vacuum) state is transferred to atmospheric pressure (normal pressure), the lid 31 may enter the container 30, and the hermeticity of the container 30 may not be ensured. Therefore, by supplying an appropriate amount of inert gas or dehumidified air by the gas supply unit, the hermeticity of the container 30 can be appropriately maintained. Furthermore, by supplying an inert gas, the preservation quality of some types of powder can be improved.

[0063] When the inert gas or dehumidified air is supplied into the reduced pressure space, the inert gas or dehumidified air permeates throughout the reduced pressure space.

[0064] When the evaluation test object is a pharmaceutical product that requires high sterility, it is preferable to use a sterilized gas as the inert gas or dehumidified air. The gas is preferably supplied so that the pressure in the reduced pressure space is 10 to 80 kPa, and more preferably 20 to 50 kPa. Supplying the gas to such a pressure can prevent the lid 31 from accidentally entering the container 30 while maintaining good sealing of the container 30.

[0065] (2) Method for extracting powder from a vacuum spray freeze drying device: The powder removal method in the vacuum spray freeze drying apparatus of the present invention is a powder removal method in the vacuum spray freeze drying apparatus that uses the powder removal device in the vacuum spray freeze drying apparatus of the present invention, and involves drying the frozen microparticles formed by the frozen microparticle formation section 40 on the receiving table 11 of the drying section 10 (hereinafter sometimes referred to as the ``drying step''), then transferring the dried powder from the receiving table 11 to a container 30 arranged in the recovery section 20 (hereinafter sometimes referred to as the ``recovery step''), and sealing the container 30 into which the powder has been placed (hereinafter sometimes referred to as the ``sealing step'').

[0066] According to this method of extracting powder in a vacuum spray freeze drying apparatus, a vacuum spray freeze drying apparatus equipped with the extraction device of the present invention can be used to efficiently and easily produce small amounts of containerized test powder having performance and properties equivalent to those of products mass-produced in a continuous vacuum freeze drying apparatus.

[0067] In the extraction method of the present invention, after sealing the container 30 with the lid 31, the inside of the vacuum spray freeze drying apparatus is returned to normal pressure (101 kPa), and the powder filled in the container 30 can be recovered.

[0068] (2-1) Drying step: In the drying step, the frozen particles formed by the frozen particle forming unit 40 are dried on the receiving platform 11 of the drying unit 10. The predetermined time for this drying can be shortened by using a vacuum spray freeze drying apparatus equipped with the take-out device of the present invention, and can be set to, for example, 1 hour or less.

[0069] (2-2) Collection step: In the collecting step, the powder dried in the drying step is poured from the receiving table 11 into the container 30 arranged in the collecting section 20. A sterilized container can be used as the container 30, and it is preferable to use a sterilized container, particularly when the evaluation test subject requires high sterility, such as a pharmaceutical product.

[0070] As explained in the above-mentioned extraction device of the present invention, the receiving table 11 can be rotated so that the surface on which the frozen particles are placed is inclined. In this way, the powder can be easily transferred from the receiving table 11 to the recovery section 20.

[0071] Fig. 4 shows the recovery section 20 having the second lifting section 29, and shows a state in which the powder is being moved from the receiving table 11 to the recovery section 20. The second lifting section 29 lifts the container 30, and the powder is recovered in the container 30. Thereafter, as shown in Fig. 5, the second lifting section 29 lowers the container 30. Then, as shown in Fig. 6, the moving section 21 moves the container 30 to the position of the lifting section 27, and thereafter, as shown in Fig. 7, the lifting section 27 lifts the container 30, and the opening of the container 30 is pressed against the lid 31 to seal it.

[0072] (2-3) Sealing step: In the plugging step, the container 30 containing the powder is plugged. The container 30 can be plugged with the lid 31 as described above in the dispensing device of the present invention. The lid 31 can be held by the lid holder as described above. By having the lid holder, the mouth of the container 30 is pressed against the lid 31, and then the container 30 is pulled down, whereby the lid 31 is released from the lid holder, and the container 30 is easily plugged.

[0073] (2-4) Gas supply step: In the extraction method of the present invention, after the powder is charged into the container 30, an inert gas or dehumidified air may be supplied into the reduced pressure space by the gas supply unit, and then the container 30 may be sealed.

[0074] There is no particular restriction on the amount of inert gas or dehumidified air supplied into this reduced pressure space, but it can be, for example, about half the atmospheric pressure or less, specifically, about 10 to 50 kPa.

[0075] An example of the inert gas is nitrogen, which is in a sterile state. By supplying an inert gas, the preservation quality of the powder can be improved depending on the type of powder. Sterilized gas can be used as the inert gas or dehumidified air, and the gas is preferably supplied so that the pressure in the reduced pressure space is 20 to 50 kPa, more preferably 20 to 40 kPa, as described above. Supplying the gas to such a pressure can prevent the lid 31 from accidentally entering the container 30, while maintaining good sealing of the container 30.

[0076] (3) Vacuum spray freeze drying equipment: One embodiment of the vacuum spray freeze drying apparatus of the present invention is a vacuum spray freeze drying apparatus 200 shown in Fig. 1. This vacuum spray freeze drying apparatus 200 includes a frozen particle forming section 40 in which droplets are sprayed into a vacuum to form frozen particles, and the powder extracting device 100 in the vacuum spray freeze drying apparatus of the present invention described above.

[0077] This vacuum spray freeze-drying apparatus 200 can efficiently and easily produce small amounts of containerized test powder that have the same performance and properties as products mass-produced by continuous vacuum freeze-drying apparatus.

[0078] (3-1) Frozen fine particle forming part: The frozen particle forming section 40 is a section in which droplets are sprayed into a vacuum to form frozen particles. Such a frozen particle forming section 40 can be appropriately adopted from a section used in a conventionally known vacuum freeze-drying device, and for example, one having a two-fluid type ultra-atomization nozzle can be used.

[0079] Since the raw materials of the test powder are valuable or expensive, the amount of droplets sprayed (amount of droplets sprayed) is small. Specifically, the droplets can be sprayed at 1 to 100 ml / min, preferably 1 to 30 ml / min, and more preferably 2 to 10 ml / min.

[0080] The vacuum is the same as that in a conventionally known vacuum freeze-drying apparatus, specifically, a pressure condition of about 0.7 kPa or less.

[0081] Furthermore, there is no particular restriction on the particle size of the frozen fine particles, but in the case of pharmaceuticals, for example, the particle size can be about 30 to 300 μm. EXAMPLES

[0082] The present invention will be specifically described below based on examples and comparative examples, but the present invention is not limited to these examples and comparative examples.

[0083] Example 1 A vacuum spray freeze-drying apparatus was prepared as shown in Figure 1. A powder was produced using this vacuum spray freeze-drying apparatus, and the powder was removed using a powder removal device.

[0084] Specifically, a small amount of containerized test powder was produced as shown in Figs. 2 to 7. First, Fig. 2 shows a state in which the container 30 is placed in a standby position to prevent contamination with undried products. Thereafter, when it is time to collect the powder in the container 30, the container 30 is moved to a powder collection position by the moving unit 21 as shown in Fig. 3. Thereafter, as shown in Fig. 4, the container 30 is raised by the second lifting unit 29, and the powder is collected in the container 30. Thereafter, as shown in Fig. 5, the container 30 is lowered by the second lifting unit 29. Then, as shown in Fig. 6, the container 30 is moved to the position of the lifting unit 27 by the moving unit 21, and then, as shown in Fig. 7, the container 30 is raised by the lifting unit 27, and the mouth of the container 30 is pressed against the lid 31 to seal it.

[0085] The test powder obtained in this manner has the same performance and properties as products mass-produced using a continuous vacuum freeze-drying apparatus, and can be used to evaluate the properties of the powder.

[0086] As described above, the vacuum spray freeze drying apparatus of Example 1 can efficiently and easily produce a small amount of containerized test powder having the same performance, properties, etc. as products mass-produced by a continuous vacuum freeze drying apparatus. The powder removal device in the vacuum spray freeze drying apparatus of Example 1 and the powder removal method using the vacuum spray freeze drying apparatus of Example 1 can efficiently and easily produce a small amount of containerized test powder having the same performance, properties, etc. as products mass-produced by a continuous vacuum freeze drying apparatus. [Industrial Applicability]

[0087] The vacuum spray freeze drying apparatus of the present invention can be used as an apparatus for producing a small amount of containerized test powder having the same performance and properties as products mass-produced by a continuous vacuum freeze drying apparatus. The powder removal device in the vacuum spray freeze drying apparatus of the present invention can be used as a component (removal device) in a vacuum spray freeze drying apparatus for producing a small amount of containerized test powder having the same performance and properties as products mass-produced by a continuous vacuum freeze drying apparatus. The powder removal method in the vacuum spray freeze drying apparatus of the present invention can be adopted as a method for removing a small amount of containerized test powder produced by the vacuum spray freeze drying apparatus. [Explanation of symbols]

[0088] 10: drying section, 11: receiving stand, 20, 120, 220: recovery section, 21: moving section, 23, 123: fixed section, 25: rod-shaped member, 27: lifting section, 27a: support, 27b: movement control section, 29: second lifting section, 30, 130: container, 31: lid, 40: frozen microparticle formation section, 100, 101, 102: powder removal device in vacuum spray freeze drying apparatus, 200: vacuum spray freeze drying apparatus.

Claims

1. a drying section connected to a frozen particle forming section in which droplets are sprayed into a vacuum at 1 to 100 ml / min to form frozen particles having a particle diameter of 30 to 300 μm; A recovery section connected to the drying section, The drying section and the recovery section form a single reduced pressure space together with the frozen particle forming section, the drying unit has a receiving stand for receiving the frozen particles formed in the frozen particle forming unit, and dries the frozen particles in a state in which the frozen particles are placed on the receiving stand to form a powder body; A powder removal device for a vacuum spray freeze drying apparatus, wherein the recovery unit has a container disposed therein, recovers the powder on the receiving table into the container, and seals the container.

2. The collection unit has a moving unit that moves the container within the collection unit, 2. The powder removal device in a vacuum spray freeze drying apparatus according to claim 1, wherein the recovery unit has a lid holding unit at its upper portion for holding a lid that seals the container, and a lifting unit for moving the container up and down to seal the container with the lid.

3. The powder removing device for a vacuum spray freeze drying apparatus according to claim 2 , wherein the moving part includes a fixing part for fixing the container.

4. 4. The powder removal device in the vacuum spray freeze drying apparatus according to claim 1, which is a part of a continuous vacuum spray freeze drying apparatus for producing powder for pharmaceutical testing.

5. The powder removal device in the vacuum spray freeze drying apparatus according to any one of claims 1 to 3, further comprising a gas supply unit that supplies an inert gas or dehumidified air into the reduced pressure space.

6. 6. The powder removal device for a vacuum spray freeze drying apparatus according to claim 5, wherein the inert gas or dehumidified air is a sterilized gas and is supplied so as to set the pressure in the reduced pressure space at 10 to 80 kPa.

7. The powder removal device for a vacuum spray freeze drying apparatus according to any one of claims 1 to 3, wherein the container is a sterilized container.

8. A method for extracting powder in a vacuum spray freeze drying apparatus using the powder extracting device in the vacuum spray freeze drying apparatus according to any one of claims 1 to 3, A method for extracting powder in a vacuum spray freeze drying apparatus, comprising drying the frozen fine particles formed by the frozen fine particle formation section on the receiving stand of the drying section, then pouring the dried powder from the receiving stand into the container arranged in the recovery section, and sealing the container into which the powder has been poured.

9. 9. The method for extracting powder in a vacuum spray freeze drying apparatus according to claim 8, wherein the receiving table rotates so that a surface for placing the frozen fine particles is inclined.

10. 9. The method for extracting powder in a vacuum spray freeze drying apparatus according to claim 8, wherein after the powder is charged into the container, an inert gas or dehumidified air is supplied into the reduced pressure space by a gas supply unit that supplies an inert gas or dehumidified air into the reduced pressure space, and then the container is sealed.

11. 11. The method for extracting powder in a vacuum spray freeze drying apparatus according to claim 10, wherein a sterilized gas is used as the inert gas or dehumidified air, and the gas is supplied so that the pressure in the reduced pressure space is 10 to 80 kPa.

12. 9. The method for extracting powder in a vacuum spray freeze drying apparatus according to claim 8, wherein a sterilized container is used as the container.

13. a frozen particle forming section in which droplets are sprayed into a vacuum to form frozen particles; A vacuum spray freeze drying apparatus comprising: a powder removal device for the vacuum spray freeze drying apparatus according to any one of claims 1 to 3.

14. 14. The vacuum spray freeze drying apparatus of claim 13, wherein the droplets are sprayed at 1 to 30 ml / min.

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