TWI618856B - Cryotrap - Google Patents

Abstract

The low-temperature trap of the present invention is a low-temperature trap provided in a casing connected to a room to be degassed, and separating low-temperature plates cooled by a mechanical freezer from a wall of the casing, and provided with a cooling separation wall The cooling and separating partition wall is in contact with one plate surface of the low-temperature plate, and separates the inside of the casing into a first space on the chamber side and a second space on the low-temperature plate side.

Description

Cryogenic trap

The present invention relates to a low-temperature trap, and more particularly, to a suitable technique for freezing and the like in a corrosion-resistant environment.

According to the industry, a vacuum drying device with a cold trap (for example, Japanese Patent No. 5574318) has been proposed in the industry to freeze and dry raw material liquids such as pharmaceuticals, foods, cosmetics, or chemicals.

According to the previous vacuum drying device, the vacuum pump is connected to the drying chamber containing the object to be dried through the exhaust path, and a cold trap is provided in the middle of the exhaust path. The dry matter can be dried by using a cold trap to condense and trap water vapor sublimated from the dry matter in the drying chamber.

In addition, as a recent trend of freeze-drying devices for pharmaceuticals, the demand for "antibody medicine" or "biomedicine" is increasing.

From the background, since these agents have higher water activity than previous chemicals, it is necessary to further reduce the water content. Therefore, in the Dayang Daily Acid News No.33 (2014) p1-p2 Mori Kojima and Yoshikura Masao “The Bio-Pharmaceutical Liquefied Nitrogen Vacuum Freeze Dryer” Internet (URL; https: //www.tn- sanso-giho.com/pdf/33/tnscgiho33_06.pdf) (hereinafter referred to as non-patent literature), a heat exchanger using liquid nitrogen is added to a vacuum freeze dryer to create a low temperature state, thereby reducing the Pressure to achieve the manufacture of pharmaceuticals.

Moreover, in the case of these drugs, it is required to manufacture the drugs without changing the manufacturing method of the clinical trial drugs.

However, if the technology disclosed in the above-mentioned non-patent literature is adopted, the device becomes extremely large due to the use of liquid nitrogen. Therefore, there is a demand for miniaturization and space saving. Furthermore, since the time, labor, and running costs of maintenance are increased due to the use of liquid nitrogen, a device and method with good operability without requiring such costs are required.

Therefore, the industry has previously studied the application of low temperature traps used in semiconductor or FPD (Flat Panel Display) manufacturing equipment to the manufacture of pharmaceuticals (for example, Japanese Patent Application Laid-Open No. 05-044642).

However, the low temperature trap was originally a device used in the manufacture of semiconductors or FPDs, and it was not envisaged to use the low temperature trap in an environment where a large amount of corrosive gas such as moisture exists. Therefore, such a low temperature trap cannot be applied as it is. Devices for pharmaceuticals.

In addition, since there are strict standards in the manufacture of pharmaceuticals and the sterilization and cleaning of the interior of the device is required, the previous small devices with high freezing capacity cannot be applied to the devices for pharmaceuticals as they are. At the same time, metals such as copper cannot be used in the parts exposed to pharmaceutical preparations, and there is a need to achieve a balance between maintaining cooling capacity and using materials for pharmaceutical manufacturing.

In addition, since the cooling capacity, temperature range, and pressure range envisioned in the manufacture of semiconductors or FPDs are different from the conditions in the manufacture of pharmaceuticals, it is not possible to apply the low temperature traps for the manufacture of semiconductors or FPDs to pharmaceuticals as they are.

The present invention has been made in view of the above circumstances, and attempts to achieve the following objects.

1. It enables high-performance freeze-drying that can be applied to the manufacture of pharmaceuticals.

2. Enable low temperature traps to be used in freeze drying (vacuum drying) devices.

3. Improve the resistance to corrosion gas.

One aspect of the present invention is a low temperature trap, which is a Inside the casing, a low-temperature trap that separates the low-temperature plates cooled by a mechanical freezer from the wall of the casing is provided with a cooling separation partition wall, which is in line with one of the above-mentioned low-temperature plates. Then, the inside of the casing is separated into a first space on the chamber side and a second space on the low-temperature plate side.

Thereby, a process such as vacuum freeze-drying in the room can be performed without exposing the low-temperature plate to the first space on the side of the room.

In the low temperature trap of one aspect of the present invention, the cooling separation partition wall has a flat plate portion closely contacting one plate surface of the low temperature plate, and a surface of the flat plate portion facing the chamber may be a well surface.

Thereby, moisture can be collected at the surface facing the chamber among the flat plate portions exposed opposite to the chamber, and the room can be degassed.

In the low temperature trap of one aspect of the present invention, the flat plate portion of the cooling separation partition wall may be connected with a cylindrical portion extending from a peripheral edge of the flat plate portion and surrounding the low temperature plate.

Thereby, the cooling separation partition wall connected to the low-temperature plate can be separated from the shell wall, and the temperature of the cooled low-temperature plate can be prevented from rising.

In the low temperature trap according to an aspect of the present invention, an exhaust mechanism may be connected to the second space on the low temperature plate side of the cooling and separating partition wall.

Thereby, the degree of vacuum of the second space (back space) can be set corresponding to the degassed space on the chamber side, and the set temperature of the low-temperature plate can be maintained.

In one aspect of the present invention, the cooling separation partition wall may be formed of a corrosion-resistant material.

Thereby, vacuum freeze-drying processing corresponding to moisture or corrosive gas can be performed.

According to one aspect of the present invention, the following effects can be exhibited: a low-temperature trap can be used even in the presence of a corrosion-resistant gas such as vacuum drying, and the true temperature can be sufficiently reduced. Moisture content of the material to be dried in air drying.

10‧‧‧Vacuum drying device

11‧‧‧ drying chamber (chamber)

11a‧‧‧Shelf

11b‧‧‧Heater (temperature control mechanism) / temperature control device

11c‧‧‧Temperature sensor

12‧‧‧The first dehydration section / dehydration section

14‧‧‧Control Unit (Control Department)

15‧‧‧Vacuum pump (the first exhaust mechanism)

16‧‧‧pump (second exhaust mechanism) / exhaust pump / vacuum pump / turbo molecular pump

17‧‧‧1st trapping device (1st trapping mechanism) / 1st cold trap

17a‧‧‧Introduction Department

17b‧‧‧Export Department

17c‧‧‧The first cooling unit / freezer

19‧‧‧Washing and sterilizing device (washing and sterilizing mechanism)

21‧‧‧The first division

21a‧‧‧ divider

22‧‧‧The first switching valve

23‧‧‧Second Division

23a‧‧‧ divider

24‧‧‧The second switching valve

26‧‧‧Pressure gauge / 1st vacuum gauge

27‧‧‧Pressure gauge / Second vacuum gauge

30‧‧‧ 2nd dehydration section / 2nd cold trap / dehydration section / low temperature trap

30A‧‧‧Degassed space (first space)

30B‧‧‧Back space (second space)

31‧‧‧shell

31c‧‧‧Back

36‧‧‧ Cooling separation wall

36a‧‧‧ Flat

36b‧‧‧Tube

36c‧‧‧Deformation Department

36d‧‧‧par

38‧‧‧trap device (trap mechanism) / second cold trap / low temperature trap

38a‧‧‧Low temperature plate / well plate

38b‧‧‧ mechanical freezer

39‧‧‧Exhaust device (exhaust mechanism)

F1‧‧‧‧Dried material / raw material / sample / degassing object

FIG. 1 is a schematic diagram showing a vacuum drying apparatus provided with a low temperature trap according to an embodiment of the present invention.

FIG. 2 is a cross-sectional view showing a low temperature trap according to an embodiment of the present invention.

FIG. 3 is a flowchart showing a vacuum drying step using a low temperature trap according to an embodiment of the present invention.

Hereinafter, a low temperature trap according to an embodiment of the present invention will be described based on the drawings.

FIG. 1 is a schematic diagram showing a vacuum drying apparatus provided with a low temperature trap according to this embodiment. In FIG. 1, reference numeral 10 denotes a vacuum drying apparatus.

The vacuum drying device 10 according to the present embodiment is used for freezing and vacuum drying a raw material liquid for manufacturing pharmaceuticals, pharmaceutical preparations, and raw materials for pharmaceuticals or pharmaceutical preparations. The object to be dried F1 is a material for a pharmaceutical preparation or a pharmaceutical preparation. The object to be dried F1 may be in a liquid state in which the above-mentioned raw material liquid is contained in a container, or may be in a solid state (for example, a block shape or a powder state) that is frozen in a vacuum in a step before the treatment using the vacuum drying device 10. In this embodiment, a case where the object to be dried F1 is a pharmaceutical preparation or a material of a pharmaceutical preparation will be described.

As shown in FIG. 1, the vacuum drying device 10 according to the present embodiment includes a drying chamber 11 that stores objects to be dried, a first dewatering unit 12 that is connected to the drying chamber 11, and a second dewatering unit 30 that is connected to the first dewatering unit 30. The dewatering section 12 is independently connected to the drying chamber 11; the first partition section 21; the second partition section 23; and the control unit 14 (control section).

The first dewatering unit 12 includes a first trapping device 17 (first trapping mechanism) capable of cooling to a first temperature, which is capable of condensing and sublimating the water sublimated from the dried object F1.

The second dewatering unit 30 includes a trap device 38 (trap mechanism), which can cool down to a temperature lower than the first temperature. The second low temperature.

The first partitioning section 21 functions as a switching device, and can selectively connect or disconnect the drying chamber 11 and the first dewatering section 12 from each other.

The second partition portion 23 functions as a switching device in the same manner as the first partition portion 21, and can selectively connect or separate the drying chamber 11 and the second dewatering portion 30 from each other.

The drying chamber 11 is a space for vacuum-drying the raw material F1 as a material to be dried. The degree of vacuum in the drying chamber 11 can be adjusted within a range of, for example, 5 to 300 Pa. The drying chamber 11 has a plurality of shelves 11a in a plurality of stages, and supports a tray (not shown) for holding the sample F1.

A heater (temperature control mechanism) 11b is provided at each of a plurality of shelves 11a in the drying chamber 11. The heater 11b is controlled by a control unit (control unit) 14 and can heat and cool the sample F1 placed on the shelf 11a. The heater 11b may be configured by a mechanism that circulates a heat medium inside the shelf 11a, or may be configured by a resistance heating type heater such as a sheathed heater. The setting temperature of the heater 11b during heating is not particularly limited, and may be set to, for example, 20 ° C.

A temperature sensor 11c is provided at at least one of the shelves 11a. The temperature sensor 11c detects the temperature of the sample F1 placed on the shelf 3 heated by the heater 11b, and outputs the detected temperature to the control unit 14 as a detection signal. Preferably, the temperature sensor 11c can measure the temperature on the upper side of the shelf 11a, and is disposed on each of the plurality of shelves 11a.

A separate first dewatering section 12 and a second dewatering section 30 are connected to the drying chamber 11, respectively, and the drying chamber 11 passes through the first dewatering section 12 and the second dewatering section 30 and a vacuum pump (first exhaust mechanism) 15 and The pump (second exhaust mechanism) 16 communicates. The vacuum pump 15 is a pump for exhausting the gas in the drying chamber 11 and setting the inside of the drying chamber 11 to a specific degree of vacuum. As the vacuum pump 15, various vacuum pumps such as a rotary pump or a dry pump can be used.

A washing and sterilizing device 19 (washing and sterilizing mechanism) is provided in the drying room 11 As described later, it is used for those who clean and sterilize the inside of the drying chamber 11, the first dewatering section 12, and the second dewatering section 30. The washing and sterilizing device 19 is controlled by the control unit 14. The washing and sterilizing device 19 can supply steam at a temperature of about 122 ° C. used for the sterilization step, or pure water that satisfies a specific standard for the washing step, into the drying chamber 11, the first dewatering section 12, and the second dewatering section 30 .

The drying chamber 11 is provided with pressure gauges 26 and 27 for measuring the pressure inside the drying chamber 11. The pressure gauge 26 is a first vacuum gauge capable of measuring the total pressure without being affected by a measurement indication value caused by the type of the measurement gas, and is a capacitance pressure gauge such as a BARATRON vacuum gauge and a diaphragm pressure gauge. The pressure gauge 27 is a vacuum gauge that can measure the total pressure by heat conduction, and is a second vacuum gauge that causes a difference in the measurement instruction value according to the type of the measurement gas, and is, for example, a Pirani vacuum gauge.

In the first drying step or heating and drying step of the first dewatering section 12, the measurement indication value of the drying chamber 11 measured by the first vacuum gauge 26 and the measurement indication value of the drying chamber 11 measured by the second vacuum gauge 27 The comparison is performed, and the point at which the difference between the measurement instruction values converges to be extremely small is judged as the end point of the first drying step or the heating and drying step. This is a discrimination step described later.

That is, when the measured values of the pressure gauges 26 and 27 are separated from each other and the measured values of the pressure gauges 26 and 27 are consistent, it is determined that the moisture in the drying chamber 11 is removed to the first dehydration unit 12. It can be switched to the second drying step of the second dewatering section 30 by the limit of the capacity. The measured values of the pressure gauges 26 and 27 are output to the control unit 14.

The first dewatering section 12 functions as one exhaust path (first exhaust path) that communicates the drying chamber 11 with the vacuum pump (first exhaust mechanism) 15. A first cold trap 17 (collecting mechanism) is provided at the first dehydration section 12. The first cold trap 17 constitutes a collection surface (first collection surface), which is capable of condensing and collecting water vapor. The first cold trap 17 is larger than the second cold trap 38 described later, and is used as a cold trap for drying, which is mainly used for trapping a larger amount of water vapor, for example.

The first cold trap 17 in the first dewatering section 12 is configured such that a pipe through which a cooling medium flows is wound in a coil shape. As a configuration other than this, the first cold trap 17 may be configured in a plate shape. The first cold trap 17 has a refrigerant introduction portion 17a and an outlet portion 17b at both ends of the tube. The introduction portion 17a and the extraction portion 17b of these refrigerants are connected to a first cooling unit 17c, which supplies the refrigerant into the first cold trap 17 and circulates the refrigerant.

The first cooling unit 17 c is controlled by the control unit 14 so that the refrigerant flows in the first cold trap 17. The first cooling unit 17c includes a compressor that compresses the refrigerant, a condenser that liquefies the compressed high-temperature and high-pressure refrigerant, an expansion valve that adiabatically expands the liquid refrigerant, and an evaporator that vaporizes the liquid refrigerant. The first cold trap 17 corresponds to the evaporator. The refrigerant is introduced into the first cold trap 17 through the introduction unit 17a and circulates through the first cold trap 17, and is led out from the outlet unit 17b for circulation. As the refrigerant, for example, Freon gas R404A or silicone oil can be used.

The first cooling unit 17c cools the surface (first collection surface) of the first cold trap 17 to a first temperature. The first temperature is a temperature at which the first cold trap 17 can condense and capture most of the water vapor in the drying chamber 11 sublimated from the sample F1. The value of the first temperature is set according to the type of the sample F1 to be dried, the reach pressure of the drying chamber, and the like. In this embodiment, it is set to about -40 ° C, about -20 ° C to -60 ° C. Range.

At the first dehydration section 12, a first partition section 21 functioning as a switching valve is provided between the drying chamber 11 and the first cold trap 17, and the first cold trap 17 and the vacuum pump (the first A first switching valve 22 is provided between the exhaust mechanisms) 15 as a switching device. The opening and closing of the first partition 21 and the first switching valve 22 are controlled by the control unit 14.

The first partitioning section 21 includes a partitioning body 21a capable of closing a portion opened on the wall surface of the drying chamber 11; a driving section (not shown) moves the partitioning body 21a; and a driving source (not shown) drives this Drive section. The driving unit is switched between a closed state where the partition body 21a is in contact with the wall surface and an open state where the partition body 21a is separated from the wall surface. The drive unit is driven and controlled by the control unit 14 to perform opening and closing control of the first partition 21. Separator 21a and drive As described later, when the first dewatering unit 12 and the drying chamber 11 are washed and sterilized, the unit is configured to be washable.

By opening the first partition portion 21, the drying chamber 11 and the first dewatering portion 12 can communicate with each other. By opening the first partition 21 and the first switching valve 22 together, the drying chamber 11 and the vacuum pump 15 can communicate with each other. The gas in the first dewatering section 12 can be discharged by closing the first partitioning section 21 and opening the first switching valve 22. The first partitioning portion 21 and the first switching valve 22 can be closed together to restrict the gas in the drying chamber 11 from being discharged through the first dewatering portion 12. The vacuum pump 15 and the first switching valve 22 constitute a first exhaust mechanism.

In the present embodiment, a second cold trap 38 is provided at the second dewatering section 30 that functions as another exhaust path (second exhaust path) communicating with the drying chamber 11. The second cold trap 38 constitutes a collection surface (second collection surface), which is capable of condensing and collecting water vapor. The second cold trap 38 is configured to be capable of being cooled to a second temperature lower than the first collection surface of the first cold trap 17.

FIG. 2 is a cross-sectional view showing a low temperature trap according to this embodiment.

The low temperature trap of the present embodiment is provided in a casing 31 as a second dehydration section 30 for final drying, and the casing 31 is connected to a drying chamber (chamber, chamber) as a degassed space installed in the vacuum drying device 10. ) 11 connection.

In this embodiment, the capacity required for the refrigerator 17c of the first cold trap 17 is to achieve a temperature adjustment of about -50 to -60 ° C, and has a large heat capacity. In contrast, the second cold trap 38 is a trap for performing secondary drying and performing a treatment after adsorbing moisture by the primary drying. Therefore, as the capability required for the second cold trap 38, it is required to achieve a further low temperature (for example, -80 ° C to -100 ° C) temperature adjustment, but the heat capacity may be small. Therefore, the second cold trap 38 is smaller than the first cold trap 17. The amount of water vapor that can be trapped by the second cold trap 38 is smaller than that of the first cold trap 17. The second cold trap 38 is used as a cold trap for final drying. For example, when the dried material contains about 500 kg of water, the first cold trap 17 dries most of the water in the dried material, and in order to dry the remaining 1% of the water in the dried material, The second cold trap 38 was used for drying.

The second cold trap 38 is controlled by the control unit 14. The low-temperature plate 38a cooled by the mechanical refrigerator 38b functions as a low-temperature trap. The second cold trap 38 is provided in the casing 31 divided by the cooling separation partition wall 36. The plate surface of the low-temperature plate member 38a is provided so as to face the deaeration object (the object to be dried) F1 in the drying chamber 11 (chamber).

As shown in FIG. 2, the cooling separation partition wall 36 is in contact with one plate surface of the low-temperature plate member 38 a. The cooling separation partition wall 36 is provided in such a manner that the space in the casing 31 is separated into the deaerated space 30A (the first space) on the drying chamber 11 side and the rear back space 30B on the low temperature plate 38a side (The second space is a space opposite to the first space with respect to the low-temperature plate member 38a). In other words, a cooling separation partition wall 36 is provided between the deaerated space 30A and the back space 30B.

As shown in FIG. 2, the cooling separation partition wall 36 has a flat plate portion 36 a which is in close contact with one plate surface of the low-temperature plate member 38 a. The surface of the flat plate portion 36a facing the drying chamber 11 (chamber) serves as the well surface of the low-temperature well.

A cylindrical portion 36b is connected to the flat plate portion 36a of the cooling separation partition wall 36 so as to extend from the periphery of the flat plate portion 36a and surround the periphery of the low-temperature plate member 38a as shown in FIG. 2. The cooling separation partition wall 36 is formed in a cylindrical shape having a bottom. The end portion of the cylindrical portion 36b is connected to the rear surface portion 31c of the case 31, so that the deaerated space 30A can be sealed. The cooling separation partition wall 36 is configured so as not to be in contact with the case 31 except for a portion where the cylindrical portion 36b is connected to the back surface portion 31c. Therefore, the vicinity of the low-temperature plate 38a can be sufficiently cooled, and the low-temperature plate 38a can function as a well plate (well surface).

Further, a rod 36d is provided between the rear surface portion 31c of the case 31 and the low-temperature plate member 38a (flat plate portion 36a). With the lever 36d, the distance between the rear surface portion 31c and the low-temperature plate member 38a is set to a specific distance.

A protruding deformed portion 36c is provided around the middle portion in the central axial direction of the cylindrical portion 36b as shown in FIG. When a pressure difference occurs between the deaerated space 30A and the back space 30B, the The portion 36c is deformed, and the cylindrical portion 36b is expandable and contractible.

The cooling separation partition wall 36 includes SUS 316 and 316L, which are well-known as corrosion-resistant materials.

Between the flat plate portion 36a and the low-temperature plate member 38a containing copper, for example, a grease or the like is arranged in order to improve the adhesion and improve the cooling efficiency. This grease is required to have high thermal conductivity, be usable at low temperatures, and low vapor pressure.

An exhaust device 39 (exhaust mechanism) is connected to the rear separation space 30B behind the cooling separation partition wall 36 facing the low-temperature plate 38a as shown in FIG. 1.

When the exhaust device 39 and the exhaust pump 16 are provided separately (when using two pumps), the same pump as the exhaust pump 16 can be used for exhaust装置 39。 Device 39. In addition, when the exhaust device 39 is not used, the exhaust pump 16 may be connected to the back space 30B, and common use of the exhaust pump may be achieved (only one exhaust pump 16 is used). In this case, the exhaust pump 16 is connected to the back space 30B via the first pipe, and the exhaust pump 16 is connected to the degassed space 30A via the second pipe. Preferably, a check valve or the like is provided in the first piping or the second piping in advance so that the gas does not flow backward from the back space 30B to the deaerated space 30A.

At the second cold trap 38, as shown in FIG. 2, in the casing 31 that becomes the second dehydration section 30, the low-temperature plate 38a frozen by the mechanical refrigerator 38b is separated from the wall of the casing 31 Set it on. In addition, the second cold trap 38 condenses water molecules and the like in the second dehydration section 30 to the low-temperature plate 38a, and maintains the water molecules and the like in the second dehydration section 30, thereby enabling water molecules in the drying chamber 11 to be condensed. And so on.

The low-temperature plate 38a can expand the helium Simon by a mechanical refrigerator 38b, and cool it to an ultra-low temperature of 80K, for example. By condensing gas molecules on the low-temperature plate 38a, the degree of vacuum in the drying chamber 11 can be increased to a high vacuum that cannot be achieved by the exhaust pump 16 or the like.

The exhaust pump 16 has a function of exhausting the inside of the deaerated space 30A in the second dehydration section 30 to a vacuum, and a turbo molecular pump can be used as the exhaust pump 16.

The second cold trap 38 cools the surface (second collection surface) of the low-temperature plate 38a to a temperature lower than the temperature of the surface of the first cold trap 17, for example, -85 in the range of -70 ° C to -100 ° C. ℃ or so. If the surface temperature of the low-temperature plate 38a is set too low, it is not preferable because the necessary mechanical freezer 38b has too much capacity. In addition, if the surface temperature of the low-temperature plate member 38a is set too high, it is not preferable because the moisture content of the dried object F1 cannot be reduced to a necessary level.

In addition, although the second cold trap 38 originally uses a high-performance low-temperature trap suitable for the manufacture of semiconductors or FPDs as described above, the second cold trap 38 can also be used under conditions that are extremely different from those generally used. WELL 38.

As shown in FIG. 1, the second dewatering section 30 is provided with a second partitioning section 23 functioning as a switching valve between the drying chamber 11 and the second cold trap 38. A second switching valve 24 as a switching mechanism is provided between the second cold trap 38 and the exhaust pump (second exhaust mechanism) 16. The opening and closing of the second partition portion 23 and the second switching valve 24 are controlled by the control unit 14.

The second partitioning section 23 includes a partitioning body 23a capable of closing a portion opened on the wall surface of the drying chamber 11; a driving section (not shown) that moves the partitioning body 23a; and a driving source (not shown) that drives this Drive section. The driving unit is switched between a closed state where the partition body 23a is in contact with the wall surface, and an open state where the partition body 23a is separated from the wall surface. The drive unit is driven and controlled by the control unit 14 to perform opening and closing control of the second partition 23. The partition body 23a and the drive unit are configured to be washable when the deaerated space 30A and the drying chamber 11 of the second dehydration unit 30 are washed and sterilized, as described later. The separator 23a is disposed closer to the object F1 to be dried in the drying chamber 11 than the orifice plate (not shown).

By opening the second partition portion 23, the deaeration space 30A of the drying chamber 11 and the second dewatering portion 30 can communicate with each other. By opening the second partition 23 and the second switching valve 24 together, the drying chamber 11 and the exhaust pump (second exhaust mechanism) 16 can communicate with each other. By closing the second partition portion 23 and opening the second switching valve 24, the gas in the deaerated space 30A of the second dewatering portion 30 can be discharged. The second partition 23 and the second switching valve 24 can be closed together. The inside of the deaeration space 30A of the second dewatering unit 30 and the drying chamber 11 are closed independently. In addition, when the gas in the degassed space 30A is exhausted, it is preferable that the gas in the back space 30B is also exhausted so that the pressures in the degassed space 30A and the back space 30B are the same. Furthermore, when the low temperature trap 38 is operated, it is necessary to exhaust the gas in the back space 30B to make the back space 30B into a vacuum state. The exhaust pump 16 and the second switching valve 24 constitute a second exhaust mechanism.

The vacuum drying device 10 according to the present embodiment cleans the drying chamber 11, the first dewatering section 12, and the second dewatering section 30, and then communicates the drying chamber 11 with the first dewatering section 12, and closes the second dewatering section 30. Perform the first freeze-drying step. Thereafter, the drying chamber 11 is communicated with the second dehydration unit 30, and the first dehydration unit 12 is closed to perform a second freeze-drying step.

Therefore, in the vacuum drying apparatus 10 of this embodiment, the deaeration space 30A of the drying chamber 11 and the first dewatering section 12 and the second dewatering section 30 can be washed and sealed separately.

Specifically, in the deaerated space 30A of the first dewatering section 12 and the second dewatering section 30, as a heat countermeasure at the time of sterilization, and for the manufacture of a pharmaceutical preparation, the partition 21a, the driving section of the partition 21a, The surfaces of the body 23a, the driving portion of the partition 23a, and the cooling and separating wall 36 may be made of metal covered with SUS, SUS 316, SUS 316L, Au, Pt, or the like. In addition, for the unwashed surface, that is, the portion not in contact with the inner surface of the dewatering portions 12 and 30, Cu with good thermal conductivity can be used.

The first switching valve 22 and the side closer to the vacuum pump 15 than the first switching valve 22 are configured so that the gas does not flow backward from the first dewatering section 12 to the drying chamber 11. Similarly, the second switching valve 24 and the side closer to the exhaust pump 16 than the second switching valve 24 are configured such that gas does not flow backward from the second dehydration section 30 toward the drying chamber 11.

In addition, the back space 30B is separated from the deaerated space 30A and adopts a structure in which gas does not flow back from the back space 30B toward the drying chamber 11 and the deaerated space 30A.

The low temperature trap is generally used to improve the heat transfer at the connection between the freezer and the trap plate, and the In foil is sandwiched between this part. In this embodiment, the In foil is changed from In foil to gold foil, and The separation by the cooling separation wall 36 prevents the In foil from being exposed to the deaerated space 30A.

The second dewatering unit 30 also uses the vacuum drying method of the present embodiment described later, and also uses the second switching valve of the second exhaust mechanism in the sterilization step, the washing step, the storage step, and the first drying step. 24 causes the exhaust pump 16 side to be blocked.

The vacuum drying method using the low temperature trap of this embodiment will be described below.

FIG. 3 is a flowchart showing a vacuum drying method using the low temperature trap of the present embodiment.

The vacuum drying method using the low temperature trap of this embodiment is shown in FIG. 3 and includes a preparation step S01, an opening and closing step S02, a sterilization step S03, a washing step S04, a preliminary drying step S05, an opening and closing step S06, and a containing step S07. Opening and closing step S08, first drying step S09, heating and drying step S10, second exhausting step S11, discrimination step S12, opening and closing step S13, second drying step S14, first exhausting step S15, closing step S16, and opening and closing step S17 And take out step S18.

The preparation step S01 shown in FIG. 3 of the vacuum drying method according to this embodiment is prepared in advance so that the object to be dried F1 can be carried into the shelf 11a. The control unit 14 prepares necessary manufacturing condition information.

Next, in the opening / closing step S02 shown in FIG. 3, each partition and valve are opened and closed by the control of the control unit 14 as follows.

Drying room 11: On

First partition 21: On

Second partition 23: On

First switching valve 22: closed

Second switching valve 24: closed

Next, the sterilization step S03 shown in FIG. 3 is in the state set in the opening and closing step S02, that is, the first compartment 21 and the second compartment 23 are opened to open the drying chamber 11 and the first dehydration unit. The 12 and the second dehydration unit 30 communicate with each other, and the steam is supplied from the washing and sterilizing device 19 by the control of the control unit 14. Thereby, the drying chamber 11 and the first dewatering unit 12 and the second dewatering unit 30 The inside of the deaerated space 30A is sterilized.

The exposed part of the pharmaceutical preparation of the dried substance F1 must be completely sterile. Therefore, each time the pharmaceutical production step is started, as a step before the pharmaceutical production step, a steam sterilization step S03 is performed. The so-called necessary sterilization in freeze-drying equipment for pharmaceuticals refers to the killing of bacteria by exposure to steam at 122 ° C or higher for 20 minutes or more.

The pressure in this steam sterilization step is set to about 210 kPa and about 220 kpa to 240 kpa. Practically speaking, as the steam sterilization step S03, the inside of the device is maintained at a high temperature for about 3 hours.

At this time, the tube of the cooling medium flowing through the first cold trap 17 is configured to be maintained at 70 ° C or lower by driving the cooling unit 17c in order to withstand this temperature.

Similarly, in order to withstand this temperature, the low-temperature plate 38a of the second cold trap 38 is configured to keep the mechanical refrigerator 38b at 70 ° C or lower by driving the mechanical refrigerator 38b while being heated. When the low temperature trap used previously receives heat transfer from the low temperature plate 38a, the heat resistance temperature of the mechanical refrigerator 38b is 70 ° C, but the temperature is maintained at the heat resistance temperature of the mechanical refrigerator 38b by the above configuration. the following. In addition, the heat resistance of the mechanical refrigerator 38b is also improved.

At this time, it is preferable that the gas in the back space 30B is also discharged by the exhaust device 39 after being separated by the cooling separation partition wall 36.

Next, the washing step S04 shown in FIG. 3 is in the state set in the opening and closing step S02, that is, the first partition 21 and the second partition 23 are opened, and the drying chamber 11 and the first dewatering section 12 and the first 2 The deaerated space 30A of the dewatering unit 30 is communicated and controlled by the control unit 14 to supply pure water that meets specific standards for washing from the washing and sterilizing device 19. Thereby, the inside of the deaeration space 30A of the drying chamber 11 and the 1st dehydration part 12 and the 2nd dehydration part 30 is wash | cleaned. Unlike vacuum devices in other manufacturing fields such as semiconductors, the inside of the device is cleaned by spraying water. Therefore, it is preferable that the drying chamber 11 and the first dewatering section 12 and the second dewatering The inside of the deaerated space 30A of the portion 30 has a structure in which water is not accumulated as much as possible.

Next, the preliminary drying step S05 shown in FIG. 3 is in the state set in the opening and closing step S02, that is, the first partition 21 and the second partition 23 are opened to open the drying chamber 11 and the first dewatering section. 12 and the deaerated space 30A of the second dewatering unit 30 communicate with each other, and the first cold trap 17 is driven by the control of the control unit 14 to the deaerated space of the drying chamber 11 and the first dewatering unit 12 and the second dewatering unit 30 30A was pre-dried and the washing water was removed. At this time, the inside of the drying chamber 11 can be heated by a temperature adjustment device (temperature adjustment mechanism) of the shelf 11a.

In the preliminary drying step S05, the control unit 14 drives the first cooling unit 17c to circulate the refrigerant in the first cold trap 17, opens the first partition 21, the second partition 23, and the first switching valve 22, and opens The second switching valve 24 is closed, and the vacuum pump 15 is driven to discharge the gas in the drying chamber 11 through the first dewatering section 12 which is the first exhaust path. As a result, the pressure in the deaerated space 30A of the drying chamber 11 and the first and second dewatering units 12 and 30 is reduced, so that the water in the interior evaporates. The vacuum pump 15 extracts the gas inside the drying chamber 11 containing water vapor, and the deaerated space 30A of the first dewatering section 12 and the second dewatering section 30 through the first exhaust path. Water vapor is collected by the first cold trap 17.

In addition, it is preferable that the second cold trap 38 is not driven in the preliminary drying step S05, but that the moisture in the deaerated space 30A of the second dewatering section 30 is after the second exhaust step S11 described later In the case of discharge in the sequential steps, etc., it is not limited.

Next, in the opening and closing step S06 shown in FIG. 3, each partition and valve are opened and closed as follows by the control of the control unit 14.

Drying room 11: On

First partition 21: On

Second partition 23: closed

First switching valve 22: closed

Second switching valve 24: closed

Next, the containment step S07 shown in FIG. 3 is the state set in the opening and closing step S06. In a state, that is, when the first partition 21 is opened to communicate the drying chamber 11 and the first dewatering section 12, and the second partition 23 is closed, the deaerated space 30A of the second dewatering section 30 is independent. In the state, the object to be dried F1 is carried into the drying chamber 11.

Next, in the opening and closing step S08 shown in FIG. 3, each partition and valve are opened and closed as follows by the control of the control unit 14.

Drying room 11: closed

First partition 21: On

Second partition 23: closed

First switching valve 22: open

Second switching valve 24: closed

Next, the first drying step S09 shown in FIG. 3 is in a state set in the opening and closing step S08, that is, when the first partition portion 21 is opened to communicate the drying chamber 11 and the first dehydration portion 12, and In a state where the second partition section 23 is closed and the second dewatering section 30 is independent, the first cold trap 17 is driven by the control of the control unit 14, and the inside of the drying chamber 11 and the first dewatering section 12 is particularly dry. The chamber 11 is freeze-dried. As a result, the pressure in the drying chamber 11 and the first dewatering unit 12 is reduced, and the water in the interior is evaporated. The vacuum pump 15 extracts the gas in the drying chamber 11 containing water vapor through the first exhaust path. Water vapor is collected by the first cold trap 17.

Non-condensable gases such as nitrogen among the gases extracted from the drying chamber 11 are not condensed at the first cold trap 17 and are extracted by the vacuum pump 15. The sample F1 placed on the shelf 11a is frozen because the latent heat of evaporation from moisture is taken away.

The temperature of the first cold trap 17 system in the first drying step S09 is set to about -40 ° C.

Next, the heating and drying step S10 shown in FIG. 3 is in a state set in the opening and closing step S08, that is, when the first partition portion 21 is opened to communicate the drying chamber 11 and the first dehydration portion 12, and the first In a state where the 2 partitioning section 23 is closed and the deaerated space 30A of the second dewatering section 30 is independent, the temperature control device installed on each shelf 11a is driven by the control of the control unit 14 11b (temperature control mechanism).

The heater (temperature-regulating mechanism) 11b accelerates the drying of the sample F1 by heating the sample F1 placed on the shelf 11a by heating the shelf 11a in the drying chamber 11 to 20 ° C. The ice contained in the heated sample F1 obtains latent heat from the sample F1, and sublimates to become water vapor.

The vacuum pump 15 extracts the gas in the drying chamber 11 containing the water vapor through the first exhaust path. Among the gases extracted by the vacuum pump 15, water vapor is condensed into ice by releasing latent heat on the surface of the first cold trap 17, and is captured by the first cold trap 17. Non-condensable gases, such as nitrogen, among the gases extracted from the drying chamber 11 are not condensed by the first cold trap 17 and are extracted by the vacuum pump 15.

By continuously exhausting the drying chamber 11 using the vacuum pump 15, the drying chamber 11 reaches the reaching pressure of the vacuum pump 15. In addition, the condensation point of the water vapor in the drying chamber 11 is lowered, so that the trapping ability of the first cold trap 17 is deteriorated, and the increase in the vacuum degree in the drying chamber 11 is stopped. When the increase in the vacuum degree in the drying chamber 11 stops, the ice contained in the sample F1 cannot be sublimated. As a result, since the sublimation is no longer performed, the ice contained in the sample F1 does not obtain latent heat from the solid raw material. Therefore, the temperature of the sample F1 rises due to the heating action of the heater 11b. The temperature sensor 11c provided on the shelf 11a detects the surface temperature of the heated sample F1 by the heater 11b, and outputs the detected temperature to the control unit 14 as a detection signal.

At the same time, the exhausting operation of the drying chamber 11 using the vacuum pump 15 is continued, and the increase in the degree of vacuum in the drying chamber 11 is stopped. At this time, the measurement instruction value of the pressure gauge 26 and the measurement instruction value of the pressure gauge 27 are output to the control unit 14, and the above-mentioned pressure gauge 26 is set to be measurable without being affected by the measurement instruction value caused by the type of the measurement gas. A first vacuum gauge of full pressure, and the above-mentioned pressure gauge 27 is a second vacuum gauge that generates a difference in measurement instruction value depending on the type of measurement gas.

The control unit 14 instructs the measurement of the drying chamber 11 measured by the first vacuum gauge 26 The value is compared with the measurement instruction value of the drying chamber 11 measured by the second vacuum gauge 27, and the time point at which the difference between the measurement instruction values converges to a minimum is detected. By comparing the difference between the measurement indication values of the first and second vacuum gauges and converging the difference between the measurement indication values to be extremely small, it is judged that the drying end point is confirmed, or the measurement indication of the second vacuum gauge The moment of the inflection point of the falling curve in the curve is detected as the drying end point confirmation.

Meanwhile, based on the detection signal from the temperature sensor 11c, the control unit 14 detects that the surface temperature of the sample F1 is the same as the heating temperature of the heater 11b and reaches the upper limit.

Secondly, the determination step S12 shown in FIG. 3 is when the control unit 14 determines that the detected drying end point is confirmed by comparing the measurement instruction values from the pressure gauges 26 and 27, and / or based on the temperature sense When it is determined that the surface temperature of the detected sample F1 and the temperature of the heater 11b have reached the same upper limit by the detection signal of the detector 11c, it is determined that this is the end point of the heating and drying step S10. In this case, first the first partition 21 is closed, and thereafter, the driving of the first cold trap 17 is stopped. After the first partition portion 21 is closed, the first switching valve 22 may be opened or closed in any state.

Next, in the opening and closing step S13 shown in FIG. 3, each partition and valve are opened and closed as follows by the control of the control unit 14.

Drying room 11: closed

The first partition 21: closed

Second partition 23: On

First switching valve 22: closed

2nd switching valve 24: open

Next, the second drying step S14 shown in FIG. 3 is in a state set in the opening and closing step S13, that is, when the second partition portion 23 is opened to degas the drying chamber 11 and the second dehydration portion 30. In a state where the space 30A is in communication, and the first partitioning section 21 is closed to make the first dewatering section 12 independent, the second cold trap 38 is driven by the control of the control unit 14 to control the drying chamber 11 and the second dewatering section 30. Inside, especially the drying chamber 11 is freeze-dried.

At this time, in order to reliably cool the low-temperature plate 38a (vacuum thermal insulation state), the exhaust space 39B is previously exhausted to a vacuum state by the exhaust device 39. The pressure state of the back space 30B is set to the same degree as the degassed space 30A.

As a result, the pressure in the deaerated space 30A of the drying chamber 11 and the second dewatering unit 30 is reduced, and the water in the interior is evaporated. The turbo molecular pump 16 extracts the gas in the drying chamber 11 containing water vapor through the second exhaust path. The water vapor is captured by the low temperature trap 38 as a second cold trap.

In addition, the heater 11b and the turbo molecular pump 16 continue to be put into a driving state after the heating and drying step S10. Alternatively, the driving of the low-temperature well 38 may be started before the second partition portion 23 is opened.

The low temperature trap 38 is set to a temperature lower than the first cold trap 17, for example, about -100 ° C.

The second cold trap 38 cooled to -100 ° C captures water vapor that cannot be captured by the first cold trap 17. Along with this, the pressure in the drying chamber 11 decreases. With this, the sublimation of the ice remaining in the sample F1 starts again. The ice remaining in the sample F1 sublimates from the sample F1, and the generated water vapor releases the latent heat on the surface of the cooling separation partition wall 36 at the position of the low-temperature plate 38a of the second cold trap 38 to condense to become ice. The second cold trap 38 is captured. With this final drying, the sample F1 dried in the heating and drying step S10 can be further dried, so that the final dryness of the sample F1 can be improved, and the water content can be reduced by two orders of magnitude. In addition, the moisture removed in the first drying step S09 and the heat drying step S10 using the first dewatering section 12 is removed in the second drying step S14 in the deaerated space 30A using the second dewatering section 30. The water content can be set to about 1%, that is, about 5kg.

Next, the sealing step S16 shown in FIG. 3 is in the state set in the opening and closing step S13, that is, when the second partition section 23 is opened to open the deaerated space 30A of the drying chamber 11 and the second dewatering section 30. In a state where the first partition 21 is closed and the first dewatering section 12 is independent, the first dewatering section 12 is controlled by the control unit 14 and a sealing device (sealing mechanism) (not shown) is used to seal the dried object F1 with aluminum. Wait for airtightness.

Next, in the opening and closing step S17 shown in FIG. 3, each partition and valve are opened and closed as follows by the control of the control unit 14.

Drying room 11: On

The first partition 21: closed

Second partition 23: closed

First switching valve 22: closed

Second switching valve 24: closed

Next, the take-out step S18 shown in FIG. 3 is to take out the dried object F1 from the drying chamber 11 after the moisture content is reduced to a desired state and the drying process is completed, and the batch of drying processes is ended.

In addition, as shown in FIG. 3, the second exhausting step S11 is part or all of the first drying step S09 and the heating and drying step S10 in a state set in the opening and closing step S08, that is, the first step The partition 21 is opened to communicate the drying chamber 11 with the first dewatering section 12, and the second partition 23 is closed to separate the deaerated space 30A of the second dewatering section 30, and the second switching valve 24 is opened. In addition, the gas in the degassed space 30A of the second dewatering section 30 in the independent state can be discharged in advance, and the moisture captured by the second cold trap 38 can be discharged to the outside. Thereby, the freeze-drying step of subsequent batches can be started without delay.

In the second exhausting step S11 of exhausting the gas in the deaerated space 30A, the exhausting device 39 can be made inoperative.

Similarly, in part or all of the second drying step S14 shown in FIG. 3, the first exhaust step S15 is in a state set in the opening and closing step S13, that is, the second partition 23 is opened. When the drying chamber 11 communicates with the deaerated space 30A of the second dewatering section 30, and the first partitioning section 21 is closed to make the first dewatering section 12 independent, the first switching valve 22 is opened, so that The gas in the first dehydration section 12 in the independent state is exhausted in advance, and the moisture trapped by the first cold trap 17 is exhausted to the outside. Thereby, the freeze-drying step of subsequent batches can be started without delay.

In this embodiment, one of the two switchable cold traps 17, 38 is set as an independent low-temperature trap 38, and the low-temperature plate 38a including the copper low-temperature trap 38 is arranged to cool and separate the components. The back wall 30B is separated after the partition wall 36, so that the dried object can be freeze-dried to reduce the moisture content by 2 orders of magnitude that could not be reached before.

In addition, compared with the previously-proposed method of obtaining extremely low temperature by using liquid nitrogen, the above-mentioned embodiment of the present invention has lower operating costs and can change the temperature conditions, so it can correspond to various drying conditions.

When the low-temperature trap 38 is activated, the first partition 21 or the second partition 23 is set to a closed state, so that the ice adhered to the first cold trap 17 can be prevented from being adsorbed at a temperature higher than the processing temperature of the first cold trap 17. Possibility of low low temperature trap 38.

Alternatively, the low-temperature plate 38a of the low-temperature trap 38 may be directly installed in the drying chamber 11 in a state separated by the cooling separation wall 36 according to the type of the object to be dried F1 or the restriction of the object to be dried F1. This configuration can be applied to, for example, a case where the product to be dried F1 is taken out in a sealed state, and the like, and ice attached to the low temperature trap 38 does not cause a problem when the product is stored.

In addition, the same freeze-drying device as the first cold trap 17 may be used to open a hole, add a valve, and add a low temperature trap 38. In this case, in order to be applicable to the washing and sterilization steps, it is necessary to set the copper low-temperature plate 38a to a specification separated by a cooling separation partition wall 36 or adopt a structure based on this.

The inside of the drying chamber 11 to which the object F1 is exposed, the inside of the first dewatering section 12 and the inside of the deaerated space 30A of the second dewatering section 30 must be completely sterile during the drying process. Therefore, each time a pharmaceutical production step is started, a steam sterilization step and a washing step must be performed as a step before the pharmaceutical production step. The so-called necessary sterilization treatment used in freeze-drying equipment for pharmaceuticals, especially for the manufacture of water for injection (WFI: water for injection), means that the bacteria are killed by exposure to steam at 122 ° C or higher for 20 minutes or more. Off.

The pressure inside the drying chamber 11 in this steam sterilization step is set to about 210 kPa and about 220 kpa to 240 kpa. Practically speaking, in the steam sterilization step of about 3 hours, the interior of the device is maintained at a high temperature. At this time, in order to withstand this temperature, the first cold trap 17 is maintained at a temperature of 70 ° C. or lower by operating the cooling unit 17 c. In order to withstand this temperature, the well of the low temperature trap 38 operates the mechanical refrigerator 38b by operating the compressor of the mechanical refrigerator 38b while being heated by steam, and operates the exhaust device 39 to maintain 70 Temperature below ℃.

In the low temperature trap 38, since the mechanical refrigerator 38b cannot be maintained for a long time in an environment exceeding 70 ° C, it is preferable to perform the sterilization treatment while the mechanical refrigerator 38b is in the running state while cooling in the sterilization step S03. In this case, since the cooling capacity of the mechanical freezer 38b is high, it is necessary to set the output of the mechanical freezer 38b so that the temperature of the trap plate 38a does not reach a sufficient temperature required for sterilization.

Moreover, if it is a device for manufacturing pharmaceutical preparations like this embodiment, the foil for improving heat transfer to the connection part of the mechanical refrigerator 38b and the low temperature plate 38a can be gold-plated foil, gold foil, etc.

At the same time, a grease or the like may be provided at a connection portion between the cooling separation partition wall 36 and the low-temperature plate member 38a, and the closeness of the cooling separation partition wall 36 and the low-temperature plate member 38a may be maintained to maintain heat transfer.

After the first drying step S09 and the heat drying step S10 where the first cold trap 17 is used to trap water at -50 ° C to -70 ° C, the second drying step S14 is further performed as a total final processing. The low temperature trap 38 absorbs the remaining moisture at -90 ° C to -100 ° C. For this reason, it is preferable to install the first cold trap 17 and the low temperature trap 38 in a cut-off room (space). In addition, it is preferable not to use the heater 11b for melting ice of the low-temperature plate 38a.

In the low temperature trap 38, the material of the cylinder portion of the mechanical refrigerator 38b includes SUS 316 and SUS 316L. The material of the cooling and separating partition wall 36 serving as the well plate is made of SUS 316 and SUS 316L, and the heat transfer part is made of a metal with high corrosion resistance such as gold foil. Make up.

The second drying step S14, which captures moisture at a very low temperature to reduce the moisture content of the dried object F1, is the final step after the first drying step S09, which is freeze-dried under normal operation, and adsorbs a very small amount of remaining Of moisture. Therefore, in the vacuum drying apparatus of this embodiment, it is not necessary to increase the processing speed and shorten the processing time, but to improve the reach of the water content by about two orders of magnitude. The low temperature trap 38 previously used in a semiconductor or FPD (flat panel display) manufacturing device is selected, and the low temperature trap 38 is applied to the vacuum drying device of this embodiment.

In addition, in the present embodiment, the surface of the cooling separation partition wall 36 (the low-temperature plate member 38a) is disposed toward the object to be dried F1, but the present invention is not limited to such an arrangement. The second dewatering unit 30 may be connected below the drying chamber 11 as long as the cooling separation partition wall 36 (the low-temperature plate 38a) is disposed so as to face the object to be dried F1, and the second dewatering unit 30 may be connected. The position of the first dewatering section 12 shown in 1 and the position of the second dewatering section 30 are changed.

(Example)

Examples of the present invention will be described below.

A specific example of the present invention will be described.

The specifications of the low temperature trap 30 in this embodiment are shown below.

Diameter r0: Ø400mm

Low temperature plate 38a thickness: 5mm

Low temperature plate 38a Material: Cu

Mechanical freezer 18c mode; G-M (Gifford-McMahon) freezer using He

Pressure change in case 31: within 30 minutes from atmospheric pressure to 13 Pa (-100 ° C)

Switch to the pressure in the drying chamber 11 at the time of the low temperature trap 38; about 1 Pa

Thickness of cooling separation wall 36: 3mm

Axial dimension of the cylindrical portion of the cooling separation partition wall 36: φ350mm

Material of cooling separation wall 36: SUS 316L

As a result of measuring the surface temperatures of the low-temperature plate 38a and the cooling separation wall 36 in such a low-temperature trap 30, it can be seen that the surface temperatures of both the low-temperature plate 38a and the cooling separation wall 36 can be stably maintained at -100. ℃.

[Industrial availability]

Examples of applications of the present invention include freeze-drying, or microorganisms (bacteria, viruses), living cells (protozoa, mammalian cell blood, etc.) which are required to reduce the moisture content of biomedicine or antibody medicine, etc. Sperm), or food-related applications.

10‧‧‧Vacuum drying device

11‧‧‧ drying chamber (chamber)

11a‧‧‧Shelf

11b‧‧‧Heater (temperature control mechanism) / temperature control device

11c‧‧‧Temperature sensor

12‧‧‧The first dehydration section / dehydration section

14‧‧‧Control Unit (Control Department)

15‧‧‧Vacuum pump (the first exhaust mechanism)

16‧‧‧pump (second exhaust mechanism) / exhaust pump / vacuum pump / turbo molecular pump

17‧‧‧1st trapping device (1st trapping mechanism) / 1st cold trap

17a‧‧‧Introduction Department

17b‧‧‧Export Department

17c‧‧‧The first cooling unit / freezer

19‧‧‧Washing and sterilizing device (washing and sterilizing mechanism)

21‧‧‧The first division

21a‧‧‧ divider

22‧‧‧The first switching valve

23‧‧‧Second Division

23a‧‧‧ divider

24‧‧‧The second switching valve

26‧‧‧Pressure gauge / 1st vacuum gauge

27‧‧‧Pressure gauge / Second vacuum gauge

30‧‧‧ 2nd dehydration section / 2nd cold trap / dehydration section / low temperature trap

30A‧‧‧Degassed space (first space)

30B‧‧‧Back space (second space)

31‧‧‧shell

36‧‧‧ Cooling separation wall

38‧‧‧trap device (trap mechanism) / second cold trap / low temperature trap

38a‧‧‧Low temperature plate / well plate

38b‧‧‧ mechanical freezer

39‧‧‧Exhaust device (exhaust mechanism)

F1‧‧‧‧Dried material / raw material / sample / degassing object

Claims (6)

A low-temperature trap is provided in a housing connected to a room that is a space to be degassed, and a low-temperature plate cooled by a mechanical freezer is separated from a wall of the housing and provided with a cooling separation wall. It is in contact with one plate surface of the low-temperature plate, and separates the inside of the housing into a first space on the chamber side and a second space on the low-temperature plate side. The cooling and separating partition wall has a surface facing the first space and The surface formed of a corrosion-resistant material has a flat plate portion which is in close contact with the plate surface of the low-temperature plate. The surface of the flat plate portion facing the chamber is a well surface. The low temperature trap of claim 1, wherein a cylindrical portion is connected to the flat plate portion of the cooling and separating partition wall, which extends from a peripheral edge of the flat plate portion and surrounds the low temperature plate. The low temperature trap of claim 2, wherein the cylindrical portion has a deformed portion that is deformed when a pressure difference occurs between the chamber and the casing. The low temperature trap according to claim 3, wherein the deformed portion is formed around the middle portion in the central axis direction of the cylindrical portion and is formed in a protruding manner. The low temperature trap according to any one of claims 1 to 4, wherein the surface on the first space side of the cooling separation partition wall is covered with SUS, SUS 316, SUS 316L, Au or Pt. The low temperature trap according to any one of claims 1 to 4, wherein an exhaust mechanism is connected to the second space on the low temperature plate side of the cooling separation wall.