KR20170008161A - Cryo trap - Google Patents

Abstract

According to the present invention, a cryo-trap is installed inside s case connected to a chamber which is a space to be separated while enabling a low-temperature panel cooled by a mechanical cooler to be spaced from a wall of the case. A plate surface of the low-temperature panel is installed to face an object to be separated inside the chamber and comprises an orifice plate installed on a front side of the plate surface.

Description

Cryotrap {CRYO TRAP}

The present invention relates to a cryotrap, and more particularly to a technique suitable for use in freeze drying.

There has been proposed a vacuum drying apparatus having a cold trap for freezing and vacuum drying a raw material liquid such as medicine, food, cosmetic, or chemical (for example, Patent Document 1).

According to the conventional vacuum drying apparatus, a vacuum pump is connected to a drying chamber containing an object to be dried through an exhaust path, and a cold trap is provided in the middle of the exhaust path. It is possible to dry the object to be dried by condensing and collecting the water vapor sublimated from the object to be dried in the drying chamber in the cold trap.

As a recent trend in freeze-drying apparatuses for medicines, there is a growing demand for " antibody medicine " or " bio medicine ".

These drugs should have a lower water content because they have higher water activity than conventional chemicals. Therefore, in the non-patent reference 1, a heat exchanger using liquid nitrogen is added to a vacuum freeze dryer to make a low-temperature state, and the pressure in the freeze-drying tank is lowered to realize the manufacture of a medicine. Further, in the case of these medicaments, it is required to prepare medicines without changing the preparation method of the test medicaments.

However, the technique described in the non-patent document 1 has a demand for miniaturization and space-saving because the apparatus becomes very large by using liquid nitrogen. In addition, the use of liquid nitrogen increases maintenance inconvenience and operation cost, and therefore, there is a demand for an apparatus and a method which do not require such a cost and are excellent in workability.

To this end, it has been investigated to use a cryotrap conventionally used in a semiconductor or FPD (Flat Panel Display) production apparatus for manufacturing a medicine (Patent Document 2).

<Prior Art Literature>

<Patent Literature>

Patent Document 1: Japanese Patent No. 5574318

Patent Document 2: Japanese Patent Application Laid-Open No. 05-044642

<Non-Patent Document 1> Daiyan Ilsan Gibo No.33 (2014) p1-p2 Morikosuke Masahiro Yonekura "Liquefied Nitrogen Vacuum Freeze Dryer for Biopharmaceuticals" Internet (URL: https://www.tn-sanso-giho.com/ pdf / 33 / tnscgiho33_06.pdf)

However, the cryotrap is a device originally used in the manufacture of semiconductors or FPDs, and the pressure range assumed in the manufacture of pharmaceuticals differs by about two orders of magnitude compared to the pressure range in the manufacture of semiconductors or FPDs. Therefore, it was impossible to apply such a cryotrap to a device for medicine.

Also, the pressure range in the manufacture of pharmaceuticals is higher than the presumed pressure in the manufacture of semiconductors or FPDs. Therefore, when the cryo-trap is applied to a device for medicines, there is a problem that sufficient cryo-trap cohesion ability can not be exhibited when the conventional cryo-trap is applied to a device for medicines as it has a large amount of moisture to be collected .

Also, the temperature range assumed in the manufacture of semiconductors or FPD differs from the temperature range in the manufacture of medicines. Therefore, it was impossible to apply such cryotrap to a device for a medicine.

SUMMARY OF THE INVENTION The present invention has been made in view of the above circumstances, and it is an object of the present invention to enable adaptation of a cryotrap to a lyophilization (vacuum drying) apparatus.

The cryotrap according to an embodiment of the present invention is a cryotrap installed in a case connected to a chamber that is a ventilation space and spaced apart from a case wall by a low temperature panel cooled by a mechanical freezer, The orifice plate is provided so as to face the object to be degassed in the chamber and provided in front of the plate surface.

Thus, the space on the chamber side and the space on the low-temperature panel side can be set to a predetermined range with respect to the orifice plate. The coagulation of water molecules or carbon dioxide molecules in a low temperature panel can be made constant even in a temperature range of about -40 to -100 DEG C, and such coagulation can be stably performed.

Specifically, when the pressure in the space on the chamber side is set to be P1 and the pressure in the space on the low-temperature panel side is set to be P2 as compared with that of the orifice plate, a critical pressure ratio satisfying the condition P2 / P1? 0.1 is set As a result, a constant exhaust speed can be realized. Here, the relationship between the pressure P2 and the pressure P1 here satisfies the condition of P1 > P2.

In the cryotrap according to an embodiment of the present invention, an interval (interval) which does not lower the aggregation amount on the plate surface can be provided between the orifice plate and the plate surface.

This makes it possible to agglomerate the aggregation amount set in the initial condition.

The cryotrap according to an embodiment of the present invention may have a plurality of openings provided in the orifice plate. Since the plurality of openings are provided in the orifice plate in this way, only the orifice conductance of the openings provided in the orifice plate is considered as the incident amount of the aggregate to the low-temperature panel surface. As a result, the critical pressure ratio can be realized, and the agglomerate can uniformly flocculate on the entire surface of the low-temperature panel.

In the cryotrap according to an embodiment of the present invention, the opening ratio of the opening in the orifice plate may be in the range of 0.8 to 0.85.

This makes it possible to stabilize the flocculation amount set in the initial condition and uniformly flocculate the agglomerate in the plane of the low temperature panel.

In the cryotrap according to an embodiment of the present invention, the opening ratio of the opening at the periphery of the orifice plate may be the same or larger than the opening ratio of the opening at the center of the orifice plate.

As a result, the agglomerate can uniformly flocculate in the plane on the entire surface of the low-temperature panel.

In the cryotrap according to an embodiment of the present invention, the shape of the opening in the orifice plate may be a shape selected from circular, polygonal, and slit shapes.

This makes it possible to realize the above critical cancer force ratio.

In the cryotrap according to an embodiment of the present invention, the shape of the opening at the periphery of the orifice plate may be the same or larger than the shape of the opening at the center of the orifice plate.

As a result, the agglomerate can uniformly flocculate in the plane on the entire surface of the low-temperature panel.

In the cryotrap according to an embodiment of the present invention, the perforator space may be connected to a vacuum drying apparatus which is a drying chamber for accommodating the laundry.

This makes it possible to sufficiently reduce the moisture content of the drying object in the vacuum drying apparatus.

According to the present invention, the cryotrap can be used for vacuum drying, and the effect of sufficiently reducing the water content of the dried product in vacuum drying can be exhibited.

1 is a schematic view showing a vacuum drying apparatus equipped with a cryotrap according to an embodiment of the present invention.
2 is a cross-sectional view illustrating a cryotrap according to one embodiment of the present invention.
3 is a front view of an orifice plate in a cryotrap according to an embodiment of the present invention.
4 is a schematic front view showing an orifice plate in a cryotrap according to an embodiment of the present invention.
5 is a flowchart illustrating a vacuum drying process using a cryotrap according to an embodiment of the present invention.
6 is a graph showing the distribution of the condensation rate in the cryotrap according to an embodiment of the present invention.

Hereinafter, a cryotrap according to an embodiment of the present invention will be described with reference to the drawings.

Fig. 1 is a schematic diagram showing a vacuum drying apparatus provided with a cryo trap according to the present embodiment. In Fig. 1, reference numeral 10 denotes a vacuum drying apparatus.

The vacuum drying apparatus 10 according to the present embodiment is used for freezing and vacuum drying the raw material liquid to produce, for example, medicines, medicines, medicaments, or medicament raw materials. The material to be dried (F1) is a material of a pharmaceutical preparation or a pharmaceutical preparation. The object to be dried F1 may be in a liquid state in which the raw material liquid is accommodated in a container and may be a solid state (for example, a lump or powder) vacuum-freezed in the previous step of the treatment using the vacuum drying apparatus 10 have. In the present embodiment, the case where the dried object F1 is a pharmaceutical agent or a pharmaceutical agent is explained.

1, the vacuum drying apparatus 10 according to the present embodiment includes a drying chamber 11 for containing a material to be dried, a first dewatering unit 12 connected to the drying chamber 11, a first dewatering unit A first partitioning part 21, a second partitioning part 23 and a control unit 14 (control part) connected to the drying chamber 11 independently from the drying chamber 11, 12,

The first dehydrating section 12 has a first collecting device 17 (first collecting device) capable of condensing and collecting the water sublimated from the article to be dried F1 and cooling it to the first temperature.

The second dewatering section 30 has a collecting device 38 (collecting means) capable of cooling to a second temperature lower than the first temperature.

The first partitioning portion 21 functions as a switching means and can selectively allow the drying chamber 11 and the first dewatering portion 12 to communicate with each other or desorb them.

The second partitioning part 23 functions as switching means like the first partitioning part 21 and can selectively allow the drying chamber 11 and the second dewatering section 30 to communicate or desorb each other.

The drying chamber (11) is a space for vacuum drying the raw material (F1) as an object to be dried. The degree of vacuum in the drying chamber 11 can be adjusted, for example, in the range of 5 to 300 Pa. The drying chamber 11 has a plurality of shelves 11a for supporting a tray (not shown) on which the sample F1 is loaded.

Each of the plurality of shelves 11a in the drying chamber 11 is provided with a heater 11b (cooling means). The heater 11b is controlled by the control unit 14 (control unit), and can heat and cool the sample F1 loaded on the shelf 11a. The heater 11b may be constituted by, for example, a mechanism for circulating the inside of the shelf 11a, or may be constituted by a resistance heating heater such as a sieve heater or the like. The set temperature of the heater 11b at the time of heating is not particularly limited, and can be set at 20 占 폚, for example.

At least one shelf 11a is provided with a temperature sensor 11c. The temperature sensor 11c senses the temperature of the sample F1 mounted on the shelf heated by the heater 11b and outputs the sensed temperature to the control unit 14 as a sensing signal. The temperature sensor 11c can measure the temperature above the shelf 11a and is preferably provided on each of the plurality of shelves 11a.

The first dewatering unit 12 and the second dewatering unit 30 are connected to the drying chamber 11 and the drying chamber 11 is connected to the first dewatering unit 12 and the second dewatering unit 30 To the vacuum pump 15 (first exhausting means) and the pump 16 (second exhausting means). The vacuum pump 15 is a pump for discharging the gas in the drying chamber 11 and for setting the inside of the drying chamber 11 to a predetermined degree of vacuum. As the vacuum pump 15, various vacuum pumps such as a rotary pump or a dry pump can be employed.

The drying chamber 11 is provided with a washing sterilizing means 19 (washing sterilizing means) for washing and sterilizing the inside of the drying chamber 11, the first dewatering portion 12 and the second dewatering portion 30 . The cleaning sterilization apparatus 19 is controlled by the control unit 14. The cleaning sterilization apparatus 19 is provided with a drying chamber 11, a first dewatering unit 12, and a second dewatering unit 30 for supplying a steam of about 122 ° C or a purified water satisfying a predetermined standard for a cleaning process, It can be supplied inside.

In the drying chamber 11, pressure gauges 26 and 27 for measuring the pressure inside the drying chamber 11 are provided. The pressure gauge 26 may be a capacitive pressure gauge, for example, a Baratron vacuum gauge or diaphragm pressure gauge, which is a first vacuum gauge capable of measuring the total pressure that is not affected by the measurement indication value depending on the type of the measurement gas. The pressure gauge 27 may be a vacuum gauge capable of measuring the total pressure using heat conduction and may be a Pirani vacuum gauge, for example, as a second vacuum gauge in which a difference in measurement indication value is generated depending on the type of the measurement gas .

The measured value in the drying chamber 11 by the first vacuum system 26 and the measured value in the drying chamber 11 by the second vacuum system 27 during the first drying process or the heating and drying process by the first dehydration section 12 And determines the convergence point at which the difference in the measurement indication value becomes very small as the end point of the first drying process or the heating and drying process. This is a determination step to be described later.

That is, when the measured values of the pressure gauges 26 and 27 are in a state in which the measured values of the pressure gauges 26 and 27 are changed to coincide with the measured values of the pressure gauges 26 and 27, It can be determined that the water has been removed to the limit and can be switched to the second drying step by the second dewatering unit 30. [ The measured values of the pressure gauges 26 and 27 are outputted to the control unit 14.

The first dehydrating section 12 functions as one exhaust path (first exhaust path) for communicating the drying chamber 11 and the vacuum pump 15 (first exhausting means). The first dehydrating section (12) is provided with a first cold trap (17). The first cold trap 17 constitutes a collecting surface (first collecting surface) capable of collecting and condensing water vapor. The first cold trap 17 is used, for example, as a cold trap for main drying, which is larger than the second cold trap 38 described later and capable of collecting more steam.

The first cold trap (17) in the first dehydration section (12) is constituted by winding a tube through which the cooling medium flows in a coil shape. As another configuration, the first cold trap 17 may be configured in the form of a plate (plate). The first cold trap 17 has a refrigerant introduction portion 17a and a lead-out portion 17b at both ends of the tube. The inlet portion 17a and the outlet portion 17b of the refrigerant are connected to the first cooling device 17c for supplying and circulating the refrigerant in the first cold trap 17.

The first cooling device 17c is controlled by the control unit 14 and circulates the refrigerant in the first cold trap 17. The first cooling device 17c has a compressor for compressing the refrigerant, a condenser for liquefying the compressed high-temperature and high-pressure refrigerant, an expansion valve for adiabatically expanding the liquid refrigerant, and an evaporator for vaporizing the liquid refrigerant. The first cold trap 17 corresponds to the above-mentioned evaporator. The refrigerant is introduced into the first cold trap 17 from the inlet portion 17a, circulated in the first cold trap 17, and circulated by being led out from the outlet portion 17b. As the refrigerant, for example, Freon gas R404A or silicone oil can be used.

The first cooling device 17c cools the surface (first trapping surface) of the first cold trap 17 to the first temperature. The first temperature is a temperature at which the first cold trap 17 is capable of collecting most of the water vapor sublimated from the sample F1 in the drying chamber 11 by condensation. The first temperature value is set according to the type of the sample F1 as the object to be dried, the arrival pressure of the drying chamber, and is in the range of about -40 DEG C to about -60 DEG C in the present embodiment.

A first partitioning part 21 functioning as a switching valve is provided between the drying chamber 11 and the first cold trap 17 in the first dewatering section 12 and the first cold trap 17, (First exhaust means) 15 is provided with a first switching valve 22 as switching means. Opening and closing of the first partitioning portion 21 and the first switching valve 22 is controlled by the control unit 14. [

The first partitioning portion 21 is provided with a partitioning member 21a capable of closing a portion opened on the wall surface of the drying chamber 11, a driving unit (not shown) for moving the partitioning member 21a, And a driving source. The driving portion switches between the closed state in which the partition body 21a contacts the wall surface and the open state in which the partition body 21a leaves the wall surface. By controlling the drive source by the control unit 14, opening / closing control of the first partitioning unit 21 is performed. The partition body 21a and the driving section are configured such that they can be cleaned when washing and sterilizing the first dehydration section 12 and the drying chamber 11 as described later.

By opening the first partitioning portion 21, the drying chamber 11 and the first dewatering portion 12 can communicate with each other. The drying chamber 11 and the vacuum pump 15 can communicate with each other by opening both the first partitioning portion 21 and the first switching valve 22. [ The gas in the first dehydration section 12 can be exhausted by closing the first partitioning section 21 and opening the first switching valve 22. [ It is possible to restrict the exhaust of the gas in the drying chamber 11 through the first dewatering section 12 by shutting off both the first partitioning section 21 and the first switching valve 22. [ The vacuum pump 15 and the first switching valve 22 constitute the first exhaust means.

The second cold trap 38 is provided in the second dewatering section 30 functioning as the other exhaust path (second exhaust path) communicating with the drying chamber 11 in the present embodiment. The second cold trap 38 constitutes a collecting surface (second collecting surface) capable of collecting the condensed water vapor. The second cold trap 38 is configured to be cooled to a second temperature lower than the first trapping surface in the first cold trap 17.

3 is a front view showing an orifice plate of the cryo-trap according to the present embodiment, and Fig. 4 is a cross-sectional view of the cryo- trap according to this embodiment. Fig. Is a schematic front view showing an orifice plate.

The cryotrap in the present embodiment is a second dewatering section 30 for finishing drying, and is connected to a drying chamber 11 (chamber) provided in the vacuum drying apparatus 10 and corresponding to a perforator space.

In the present embodiment, the capacity required of the freezer 17c of the first cold trap 17 is such that the temperature can be regulated in the vicinity of -50 to -60 占 폚 and has a large heat capacity. On the other hand, the second cold trap 38 is used for secondary drying, and is a device for performing the treatment after the moisture in the primary drying furnace is adsorbed. For this purpose, the second cold trap 38 is required to have a capability of realizing adjustment of a lower temperature (for example, from -80 DEG C to -100 DEG C), but the heat capacity may be small. For this purpose, 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 finish drying. For example, when the object to be dried contains about 500 kg of water, the first cold trap 17 dries most of the moisture of the object to be dried, and in order to dry the remaining 1% 2 cold trap 38 is used.

The second cold trap 38 is controlled by the control unit 14 and has a low temperature panel 38a cooled by the mechanical freezer 38b. The low temperature panel 38a functions as a cryotrap.

2 and 3, a low-temperature panel 38a, which is frozen by a mechanical freezer 38b, is provided in a case 31 constituting the second dewatering section 30. As shown in Fig. Water molecules or carbon dioxide molecules are condensed in the low temperature panel 38a in the second dewatering section 30 so that these molecules are held in the second dewatering section 30. [ That is, the second cold trap 38 is configured to reduce water molecules, carbon dioxide molecules, and the like in the drying chamber 11.

The low-temperature panel 38a is disposed in the second dehydrating section 30 so as to be spaced apart from the case 31 serving as the wall surface of the second dehydrating section 30. [ The plate surface of the low-temperature panel 38a is provided so as to face the object to be degassed F1 (object to be dried) in the drying chamber 11 (chamber). An orifice plate 33 is provided forward (on the article to be dried F1 side) of the plate surface of the low temperature panel 38a. In other words, the orifice plate 33 is disposed in the second dehydrating section 30 so as to be positioned between the drying chamber 11 and the low-temperature panel 38a.

The orifice plate 33 is disposed so as to cover the entire surface of the low temperature panel 38a when viewed from the object F1 toward the orifice plate 33. [ Specifically, the orifice plate 33 can be provided so that the entire opening located on the side of the drying chamber 11 of the cylindrical case 31 is mostly covered. At this time, the orifice plate 33 is disposed so as not to be in contact with the case 31, and four positions, for example, are fixed by the pins 31a protruding inward from the case 31. [

The distance d between the orifice plate 33 and the low temperature panel 38a is set to an interval that does not lower the aggregation amount of water molecules or carbon dioxide molecules that are coagulated by the low temperature panel 38a have.

Specifically, the distance d is set so as to be within an average free path of water molecules with respect to the pressure P2 in the space on the side of the low temperature panel 38a than the orifice plate 33. [ For example, the distance d is set so that the low temperature panel 38a has the ability to capture such necessary trapped water amount corresponding to the above-mentioned coagulation amount, that is, the required trapped water amount.

Specifically, in the case of a device operating condition in which the temperature in the vicinity of the low-temperature panel 38a is about -100 DEG C and the pressure is 1 to 10-3 Pa, the distance d can be set to about 1 to 100 mm.

The orifice plate 33 is provided with a plurality of openings 34 as shown in Figs.

This opening 34 can be set so that the average opening ratio in the entire surface of the orifice plate 33 is in the range of 0.8 to 0.85.

4, the central portion 33c, which is a region having the radius r1 in the orifice plate 33, and the central portion 33c in the orifice plate 33, The opening ratio of the opening 34 of the peripheral portion 33r which is an area from the radius r1 to the radius r2 of the electrode 33 is different. Concretely, the opening ratio of the opening 34 of the orifice plate 33 can be set so that the opening ratio of the peripheral edge portion 33r is equal to or larger than the opening ratio of the center portion 33c. Thus, the coagulation amount of water molecules or carbon dioxide molecules on the plate surface of the low-temperature panel 38a can be set to be uniform on the surface of the low-temperature panel 38a. Therefore, water molecules or carbon dioxide molecules can be efficiently agglomerated on the side surface or the back surface side of the low-temperature panel 38a, and such aggregation can be effectively performed.

The outline shape of the opening 34 of the orifice plate 33 may have a circular shape as shown in Fig. 3, and may have a shape selected from a polygonal shape, a slit shape, and a mesh shape.

4, the shape of the opening 34 in the peripheral edge portion 33r is set to be equal to or larger than the shape of the opening 34 in the central portion 33c . At this time, the shape of the opening 34 in the center portion 33c and the shape of the opening 34 in the peripheral edge portion 33r may be similar to each other.

That is, for example, when the outline shape of the opening 34 is circular, the diameter of the opening 34 of the peripheral edge portion 33r is set to be equal to or larger than the diameter dimension of the opening 34 at the center portion 33c .

This makes it possible to set the coagulation of water molecules or carbon dioxide molecules on the plate surface of the low-temperature panel 38a to be uniform in the in-plane direction of the low-temperature panel 38a. Therefore, water molecules or carbon dioxide molecules can be efficiently agglomerated on the side surface or the back surface side of the low-temperature panel 38a, and such aggregation can be effectively performed.

The shape and arrangement of the openings 34 of the orifice plate 33 are set such that the pressure in the space on the side of the drying chamber 11 (chamber) is set to P1 rather than the pressure of the orifice plate 33, Quot; P2 / P1 &quot; 0.1 when the pressure in the space on the side of the &quot; L &quot; As a result, a constant exhaust speed can be realized. The relationship between the pressure P2 and the pressure P1 here satisfies the condition of P1 &gt; P2.

The low temperature panel 38a can be cooled to a cryogenic temperature of, for example, 80K by the mechanical freezer 38b by simally expanding the helium gas. By condensing gas molecules in the low-temperature panel 38a, the degree of vacuum in the drying chamber 11 can be increased to a high vacuum that can not reach the exhaust pump 16 or the like.

The exhaust pump 16 has a function of evacuating the inside of the second dewatering unit 30 in vacuum, and a turbo molecular pump can be used as the exhaust pump 16.

The second cold trap 38 is disposed between the surface of the low temperature panel 38a (second collecting surface) and the surface of the first cold trap 17 at a temperature lower than the surface temperature of the first cold trap 17, for example, about -70 ° C to -100 ° C, Lt; 0 &gt; C. If the surface temperature of the low temperature panel 38a is set too low, the capacity of the necessary mechanical refrigerator 38b becomes too large. If the surface temperature of the low-temperature panel 38a is set too high, the water content of the object to be dried F1 can not be reduced to a required level.

Further, although the second cold trap 38 uses a high-performance cryo-trap which can be applied to manufacture semiconductors or FPDs as described above, the second cold trap 38 may be provided in a very different condition than a conventionally used condition. It can also be used.

In the second dewatering section 30, a second partitioning section 23 functioning as a switching valve is provided between the drying chamber 11 and the second cold trap 38. A second switching valve 24 as switching means is provided between the second cold trap 38 and the exhaust pump 16 (second exhausting means). The opening and closing of the second partitioning part 23 and the second switching valve 24 are controlled by the control unit 14.

The second partitioning portion 23 includes a partitioning member 23a capable of closing a portion opened on the wall surface of the drying chamber 11, a driving unit (not shown) for moving the partitioning member 23a, and a driving source I have. The driving portion switches between the closed state in which the partition body 23a contacts the wall surface and the open state in which the partition body 23a separates from the wall surface. By controlling the drive source by the control unit 14, opening / closing control of the second partition part 23 is performed. The partition body 23a and the driving section are configured to be cleanable when washing and sterilizing the second dewatering section 30 and the drying chamber 11, as described later.

The partition body 23a is disposed at a position closer to the object to be dried F1 of the drying chamber 11 than the orifice plate 33. [

By opening the second partition portion 23, the drying chamber 11 and the second dewatering portion 30 can communicate with each other. The drying chamber 11 and the exhaust pump 16 (second exhaust means) can be communicated with each other by opening both the second partition portion 23 and the second switching valve 24. The gas in the second dehydration section 30 can be evacuated by closing the second partition section 23 and opening the second switching valve 24. [ The inside of the second dehydrating section 30 and the drying chamber 11 can be closed independently by closing both the second partitioning section 23 and the second switching valve 24. The exhaust pump 16 and the second switching valve 24 constitute a second exhausting means.

The vacuum drying apparatus 10 according to the present embodiment is configured such that the drying chamber 11, the first dewatering unit 12 and the second dewatering unit 30 are cleaned and then the drying chamber 11 and the first dewatering unit 12 The second dewatering section 30 is closed and the first lyophilization process is performed. Thereafter, the drying chamber 11 and the second dewatering section 30 are communicated with each other, the first dewatering section 12 is closed, and the second freeze-drying process is performed.

To this end, in the vacuum drying apparatus 10 according to the present embodiment, the drying chamber 11, the first dehydrating section 12, and the second dehydrating section 30 can be cleaned and sealed, respectively.

Specifically, in the first dewatering section 12 and the second dewatering section 30, a partitioning body 21a, a drive part of the partitioning body 21a, a partitioning body 23a, The surface of the drive section of the partition body 23a and the low temperature panel 38a (cryotrap) may be covered with a metal such as SUS, SUS316, Au, or Pt. Further, copper which is not cleaned, that is, a portion that does not contact the inner surface of the dewatering portion 12, 30 and which has good heat transfer can be used.

The gas does not flow back from the first dewatering section 12 to the drying chamber 11 in the case of the side of the vacuum pump 15 rather than the first switching valve 22 and the first switching valve 22. [ Similarly, in the case of the exhaust pump 16 side rather than the second switching valve 24 and the second switching valve 24, the gas does not flow back from the second dewatering section 30 to the drying chamber 11.

The cryotrap is usually made of indium foil, gold-plated, gold-plated, etc., in the connection between the refrigerator and the trap panel, with indium foil interposed therebetween to improve thermal conductivity.

In the case of the sterilization step, the cleaning step, the receiving step and the first drying step in the vacuum drying method of this embodiment, which will be described later, in the second dewatering section 30 of the second dewatering section 30, The side of the exhaust pump 16 is closed.

Hereinafter, a vacuum drying method using the cryotrap in the present embodiment will be described.

5 is a flowchart showing a vacuum drying method using the cryotrap in the present embodiment.

The vacuum drying method using the cryo-trap according to the present embodiment includes a preparation step (S01), an opening and closing step (S02), a sterilization step (S03), a cleaning step (S04), a preliminary drying step (S05) (S06), an accommodating process (S07), an opening and closing process (S08), a first drying process (S09), a heating and drying process (S10), a second evacuation process (S11), a discriminating process (S13), a second drying step (S14), a first evacuation step (S15), a sealing step (S16), an opening and closing step (S17) and a taking-out step (S18).

As shown in Fig. 5, the vacuum drying method of the present embodiment is prepared so that the dried object F1 necessary for the preparation step (S01) can be loaded into the shelf 11a. Further, necessary manufacturing condition information in the control unit 14 is prepared.

Next, in the opening and closing step (S02) shown in Fig. 5, each partition and valve is opened and closed as controlled by the control unit 14 as follows.

Drying room (11): open

First partition 21: Open

Second partition (23): open

First switching valve 22: Closed

Second switching valve 24: Closed

5 (S03), the first partitioning part 21 and the second partitioning part 23 are opened to open the drying chamber 11, the first partitioning part 21 The dehydrating section 12 and the second dehydrating section 30 are communicated with each other and the steam is supplied from the washing sterilizing means 19 under the control of the control unit 14. [ Thus, the interior of the drying chamber 11, the first dewatering unit 12 and the second dewatering unit 30 is sterilized.

The exposed part of the drug product (F1) must be completely sterile. For this purpose, the steam sterilization step (S03) is carried out as a step before the pharmaceutical production process every time the pharmaceutical production process is started. The necessary sterilization in the freeze-drying device for medicines is to expose the microorganism to the microorganisms by exposing the microorganisms to a vapor of 122 占 폚 or more for 20 minutes or more.

The pressure in the steam sterilization step is about 210 kPa and about 220 kPa to 240 kPa. Actually, as the steam sterilization step (S03), the inside of the equipment is maintained at a high temperature for about 3 hours.

At this time, the tube through which the cooling medium of the first cold trap 17 flows is configured to maintain 70 ° C or lower by driving the cooling device 17c to withstand the temperature.

The low temperature panel 38a of the second cold trap 38 is structured such that the mechanical refrigerator 38b is maintained at 70 deg. C or lower by driving the mechanical refrigerator 38b during heating so as to withstand the temperature have. When the heat from the low temperature panel 38a is transmitted to the cryoprene in the past, the heat resistance temperature of the mechanical freezer 38b is 70 deg. C, but it can be kept below the heat resistant temperature of the mechanical refrigerator 38b. In addition, heat resistance of the mechanical refrigerator 38b can be improved.

Next, as the cleaning step (S04) shown in Fig. 5, the first partitioning portion 21 and the second partitioning portion 23 are opened, The dehydrating section 12 and the second dehydrating section 30 are communicated with each other and the purified water satisfying a predetermined standard is supplied from the washing sterilizing means 19 for cleaning by the control of the control unit 14. [ Thus, the inside of the drying chamber 11, the first dewatering unit 12, and the second dewatering unit 30 are cleaned. Unlike vacuum devices in other manufacturing fields such as semiconductors, water is sprayed inside the device and cleaned. To this end, it is preferable that the inside of the drying chamber 11, the first dewatering unit 12 and the second dewatering unit 30 are not soiled with water.

Next, as the preliminary drying step (S05) shown in Fig. 5, the state set in the opening and closing step (S02), i.e., the state in which the first partitioning part 21 and the second partitioning part 23 are opened and the drying chamber 11, 1 dewatering unit 12 and second dewatering unit 30 are communicated with each other to drive the first cold trap 17 under the control of the control unit 14 to control the drying chamber 11 and the first dewatering unit 12, 2 Dewatering section 30 is preliminarily dried and cleansing water is removed. At this time, the inside of the drying chamber 11 can be heated by the cooling device (cooling means) of the shelf 11a.

In the preliminary drying step (S05), the control unit 14 drives the first cooling device 17c to circulate the refrigerant into the first cold trap 17, and the first partition 21, The first switching valve 22 is opened and the second switching valve 24 is closed to drive the vacuum pump 15 so that the gas in the drying chamber 11 is discharged to the first exhaust path 1 &lt; / RTI &gt; As a result, the pressures of the drying chamber 11, the first dewatering unit 12 and the second dewatering unit 30 are lowered, and the moisture inside is evaporated. The vacuum pump 15 discharges the gas inside the drying chamber 11, the first dewatering unit 12 and the second dewatering unit 30 including steam through the first exhaust path. The water vapor is collected in the first cold trap 17.

It is preferable that the second cold trap 38 is not driven in the preliminary drying step (S05), but the moisture in the second dewatering section (30) is subjected to a post-process And the like.

Next, in the opening and closing step (S06) shown in Fig. 5, each partition and the valve are opened and closed as follows by the control of the control unit 14. [

Drying room (11): open

First partition part (21): open

Second partition part 23: Closed

First switching valve 22: Closed

Second switching valve 24: Closed

Next, as the receiving step (S07) shown in Fig. 5, the state set in the opening and closing step (S06), i.e., the state in which the first partitioning part (21) is opened to make the drying chamber (11) and the first dewatering part And the laundry F1 is carried into the drying chamber 11 while the second partitioning portion 23 is closed and the second dewatering portion 30 is made independent.

Next, in the opening and closing step (S08) shown in Fig. 5, each partition and the valve are opened and closed by the control of the control unit 14 as follows.

Drying room (11): Closed

First partition part (21): open

Second partition part 23: Closed

First switching valve 22: opened

Second switching valve 24: Closed

5, the first partitioning portion 21 is opened to open the drying chamber 11 and the first dewatering portion 12 in the state set in the opening / closing step (S08), that is, The first cold trap 17 is driven under the control of the control unit 14 in a state in which the second partitioning part 23 is closed and the second dewatering part 30 is made independent, And the inside of the first dehydrating section 12, particularly the drying chamber 11, are freeze-dried. As a result, the pressures of the drying chamber 11 and the first dewatering section 12 are lowered, and the water content therein evaporates. The vacuum pump 15 discharges the gas in the drying chamber 11 containing water vapor through the first exhaust path. The water vapor is collected in the first cold trap 17.

The non-condensed gas such as nitrogen in the gas discharged from the drying chamber 11 is discharged from the vacuum pump 15 without condensation in the first cold trap 17. The sample F1 loaded on the shelf 11a is frozen by depriving latent heat of evaporation from moisture.

The temperature of the first cold trap 17 in the first drying step (S09) is set to about -40 deg.

5, the first partitioning portion 21 is opened to connect the drying chamber 11 and the first dewatering portion 12 to each other in the state set in the opening and closing process (S08) The cooling unit 11b installed on each shelf 11a under the control of the control unit 14 while the second partitioning unit 23 is closed and the second dewatering unit 30 is made independent, ) (Cooling means).

The heater (heating means) 11b heats the sample F1 mounted on the shelf 11a by heating the shelf 11a in the drying chamber 11 to 20 占 폚 to accelerate the drying of the sample F1. The ice contained in the heated sample F1 absorbs latent heat from the sample F1 and sublimates to become steam.

The vacuum pump 15 discharges the gas in the drying chamber 11 containing the water vapor through the first exhaust path. The vapor in the gas discharged by the vacuum pump 15 is trapped by the first cold trap 17 by releasing latent heat from the surface of the first cold trap 17 and condensing to ice. The non-condensed gas such as nitrogen in the gas discharged from the drying chamber 11 is discharged by the vacuum pump 15 without condensation in the first cold trap 17.

By continuing the evacuation operation in the drying chamber 11 by the vacuum pump 15, the drying chamber 11 reaches the reaching pressure of the vacuum pump 15. Further, as the condensation point of the water vapor in the drying chamber 11 is lowered, the trapping ability of the first cold trap 17 deteriorates, and the rise of the degree of vacuum in the drying chamber 11 stops. When the rise of the degree of vacuum in the drying chamber 11 is stopped, the ice contained in the sample F1 can not sublimate. As a result, the ice contained in the sample F1 can not absorb the latent heat from the solid raw material, and 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 senses the surface temperature of the sample F1 heated by the heater 11b and outputs the sensed temperature to the control unit 14 as a sensing signal.

At the same time, the evacuation operation of the drying chamber 11 by the vacuum pump 15 is continued, and the rise of the degree of vacuum in the drying chamber 11 is stopped. At this time, as a vacuum gauge capable of measuring the measurement command value of the pressure gauge 26, which is the first vacuum gauge capable of measuring the total pressure without being influenced by the measurement instruction value depending on the type of the measurement gas, and the total pressure using the thermal conduction, And outputs the measurement instruction value of the pressure gauge 27, which is the second vacuum system in which a difference occurs in the measurement instruction value depending on the kind of the measurement gas, to the control unit 14. [

The control unit 14 compares the measurement instruction value in the drying chamber 11 by the pressure gauge 26 as the first vacuum system with the measurement instruction value in the drying chamber 11 by the second vacuum system 27, And detects a convergence point at which the difference between the indicated values becomes very small. By comparing the difference between the measurement instruction values of the first and second vacuum systems 26 and 27 and determining that the convergence point at which the difference in the measurement instruction value becomes very small is determined at the time of confirming the end point of the drying, The inflection point of the descending curve in the measurement instruction curve is detected when confirming the drying end point.

At the same time, the control unit 14 detects that the surface temperature of the sample F1 becomes equal to the heating temperature of the heater 11b and reaches the limit, based on the detection signal from the temperature sensor 11c.

5, the control unit 14 compares the measurement indications from the pressure gauges 26, 27 to determine the end point of dry separation and / or the temperature sensor 11c It is determined that the surface temperature of the sample F1 is equal to the temperature of the heater 11b and reaches the limit time point. In this case, the first partition part 21 is first closed, and then the driving of the first cold trap 17 is stopped. Further, if the first partitioning portion 21 is closed, the first switching valve 22 may be open or closed.

Next, in the opening and closing step (S13) shown in Fig. 5, each partition and valve is opened and closed as follows by the control of the control unit 14. [

Drying room (11): Closed

First partition part (21): Closed

Second partition part 23: Open

First switching valve 22: Closed

Second switching valve 24: Open

Next, in the second drying step (S14) shown in Fig. 5, the state set in the opening and closing step (S13), i.e., the state in which the second partition 23 is opened to make the drying chamber 11 and the second dewatering section 30 communicate The second cold trap 38 is driven under the control of the control unit 14 in a state in which the first partition part 21 is closed and the first dehydration part 12 is made independent, 2 The inside of the dewatering unit 30, particularly the drying chamber 11, is freeze-dried.

As a result, the pressures of the drying chamber 11 and the second dewatering section 30 are lowered, and the water content therein evaporates. The turbo molecular pump 16 discharges the gas in the drying chamber 11 containing water vapor through the second exhaust path. The water vapor is trapped by the cryotrap 38, which is the second cold trap.

At the same time, the pressure P1 in the space on the side of the drying chamber 11 and the pressure P2 pressure in the space on the low-temperature panel 38a side are controlled by the orifice plate 33 to P2 (on the low-temperature panel 38a side (The pressure on the side of the drying chamber 11) &lt; / = 0.1 and the condition P1 &gt; P2. Thus, the stable cryotrap 38 can realize a stable and constant exhaust velocity.

At this time, water (water molecules) uniformly flocculate in the surface of the low-temperature panel 38a on the surface of the low-temperature panel 38a on the side of the drying chamber 11 so that the distance between the orifice plate 33 and the low- it is possible to agglomerate the ice on the surface of the low-temperature panel 38a so that the space of the low-temperature panel 38a is filled. In addition, ice can be agglomerated on the back surface of the low-temperature panel 38a. In addition, the orifice plate 33 need not be cooled like the low-temperature panel 38a, but may be cooled.

In addition, the heater 11b and the turbo molecular pump 16 are in a state of continuing to drive from the heating and drying step (S10). Further, the driving of the cryotrap 38 can be started before the second partition portion 23 is opened.

The cryotrap 38 is set to a lower temperature than the first cold trap 17, for example, about -100 degrees Celsius.

The second cold trap 38 cooled to -100 ° C. collects the water vapor that could not be trapped in the first cold trap 17. The pressure of the drying chamber 11 is lowered. As a result, the sublimation of the ice remaining in the sample F1 resumes. The ice remaining in the sample F1 absorbs the latent heat from the sample F1 and sublimates. The generated water vapor releases latent heat to the surface of the low-temperature panel 38a of the second cold trap 38, And is collected by the second cold trap 38. By such finishing drying, the sample F1 subjected to the heating and drying step (S10) can be further dried, and the final drying degree of the sample (F1) can be increased to lower the moisture content by two orders of magnitude. Moreover, the moisture removed in the first drying step (S09) and the heating drying step (S10) using the first dewatering section (12) is removed in the second drying step (S14) using the second dewatering section The water content may be about 1%, that is, about 5 kg.

Next, as a sealing step (S16) shown in Fig. 5, a state set in the opening and closing step (S13), that is, a state in which the second partition part 23 is opened to make the drying chamber 11 and the second dewatering part 30 communicate (Airtight means) (not shown) under the control of the control unit 14 in a state in which the first partitioning portion 21 is closed and the first dehydrating portion 12 is made independent, F1) is sealed with an aluminum paint or the like.

Next, in the opening and closing step (S17) shown in Fig. 5, each partition and the valve are opened and closed by the control of the control unit 14 as follows.

Drying room (11): open

First partition part (21): Closed

Second partition part 23: Closed

First switching valve 22: Closed

Second switching valve 24: Closed

Next, as a take-out step (S18) shown in Fig. 5, the dry matter (F1) whose moisture content has decreased to a desired state and has undergone the drying treatment is taken out from the drying chamber (11) And terminates.

5, in a part or all of the first drying step (S09) and the heating and drying step (S10), the state set in the opening and closing step (S08) as the second evacuation step (S11) The first partitioning part 21 is opened so that the drying chamber 11 and the first dewatering part 12 are communicated with each other and the second partitioning part 23 is closed to make the second dewatering part 30 independent. 2 switching valve 24 is opened and the gas of the second dewatering unit 30 which is in an independent state is exhausted, moisture collected in the second cold trap 38 can be discharged to the outside. As a result, the freeze-drying process for the next batch can be started without delay.

In the part or all of the second drying step (S14) shown in Fig. 5, the state set in the opening and closing step (S13) as the first exhausting step (S15), that is, the second partitioning part The first switching valve 22 is opened in a state in which the drying chamber 11 and the second dewatering section 30 are communicated with each other and the first partitioning section 21 is closed and the first dewatering section 12 is made independent , The gas in the first dehydrating section 12 which is in an independent state can be exhausted, and the moisture trapped in the first cold trap 17 can be discharged to the outside. As a result, the freeze-drying process of the next batch can be started without delay.

In this embodiment, one of the two switchable cold traps 17 and 38 is used as an independent cryotrap 38, and the orifice plate 33 is provided, It has become possible to freeze dry the laundry to a low moisture content.

Further, since the maintenance cost is lower than the conventionally proposed method of obtaining cryogenic temperature by liquid nitrogen and the temperature condition is also variable, it is possible to cope with various drying conditions.

When the cryotrap 38 is started, the first partition 21 or the second partition 23 is closed so that the cryotrap 38 having a lower processing temperature than the first cold trap 17 It is possible to prevent the ice attached to the first cold trap 17 from being adsorbed.

Another partitioning valve may be provided between the cryotrap 38 and the drying chamber 11 so as not to damage the function of the orifice plate 33 in addition to the second partitioning portion 23.

Temperature panel 38a in the cryotrap 38 while maintaining a predetermined positional relationship capable of maintaining the above-described critical pressure ratio, depending on the kind of the object to be dried F1 or the restriction by the object F1 to be dried. And the orifice plate (33) can be installed directly in the drying chamber (11). The above configuration is applicable to a case in which ice adhered to the cryotrap 38 such as a product such as a product in which the object to be dried F1 is hermetically removed is not a problem at the time of delivering the product.

Further, it is possible to add a valve and to add a cryotrap 38 to the already installed freeze-drying device by perforating a hole like the first cold trap 17. In this case, it is necessary to adopt the above-mentioned specification or a configuration similar to the above in order to be applicable to the cleaning sterilization process.

The inside of the drying chamber 11 in which the object to be dried F1 is exposed, the inside of the first dehydrating section 12 and the inside of the second dehydrating section 30 must be completely sterilized in the drying process. For this purpose, it is essential to carry out the steam sterilization process and the cleaning process as the preceding process of the pharmaceutical production process every time the pharmaceutical production process is started. The necessary sterilization treatment in the freeze-drying apparatus used for the production of pharmaceuticals, particularly water for injection (WFI), is to kill bacteria by exposure to steam of 122 占 폚 or more for 20 minutes or more.

The pressure inside the drying chamber 11 in the steam sterilization step is about 210 kPa and about 220 kPa to 240 kPa. In fact, the steam sterilization process takes about 3 hours, and the inside of the apparatus is maintained at a high temperature. At this time, the first cold trap 17 operates the cooling device 17c to withstand a high temperature to maintain a temperature of 70 ° C or lower. Further, when the steam is heated, the compressor of the mechanical refrigerator 38b is driven to maintain the temperature of 70 DEG C or less so that the trap of the cryotrap 38 can withstand the high temperature.

The mechanical freezer 38b can not be maintained for a long period of time in an environment exceeding 70 DEG C so that the mechanical freezer 38b is cooled during operation and sterilized during the sterilization process S03 . In this case, it is necessary to set the output of the mechanical freezer 38b such that the cooling capacity of the mechanical freezer 38b is high and the temperature of the trap panel 38a reaches a temperature sufficient for sterilization.

In addition, in the apparatus for producing a medicinal preparation as in the present embodiment, the object to improve the thermal conductivity at the connection portion between the mechanical refrigerator 38b and the low-temperature panel 38a can be gold-plated, gold-plated or the like.

After completion of the first drying step (S09) and the heat drying step (S10) in which water is trapped by the first cold trap (17) at -50 DEG C to -70 DEG C, The second drying step (S14) for squeezing out the remaining water by the cryotrap 38 at a temperature of 40 DEG C is carried out. For this purpose, it is preferable that the first cold trap 17 and the cryotrap 38 are installed in a separate room (space). It is preferable that the heater 11b is not used for the melting of the low temperature panel 38a.

The material of the cylinder portion of the mechanical freezer 38b in the cryo trap 38 is made of SUS316. The material of the low-temperature panel 38a (trap panel) portion is made of SUS316, and the heat-conducting portion is made of metal having high corrosion resistance such as gold leaf.

The second drying step (S14) for trapping moisture at a cryogenic temperature and lowering the water content of the object to be dried (F1) is a finishing step after the first drying step (S09) in which freeze drying is performed by a normal operation, do. Therefore, in the vacuum drying apparatus of the present embodiment, it is not necessary to increase the processing speed and shorten the processing time, and to improve the degree of water content by about two orders of magnitude. Conventionally, the cryotrap 38 used in a semiconductor or FPD (flat panel display) manufacturing apparatus is selected and the cryotrap 38 is used in the vacuum drying apparatus of the present embodiment.

In the present embodiment, the surfaces of the orifice plate 33 and the low temperature panel 38a are disposed so as to face the laundry F1, but the present invention is not limited to this arrangement. If the orifice plate 33 and the low temperature panel 38a are disposed so as to face the object to be dried F1 and the orifice plate 33 can be disposed so that the condition of the above-described critical pressure ratio P1 / P2 is satisfied, 2 dewatering unit 30 may be connected to the lower side of the drying chamber 11 and the position of the first dewatering unit 12 and the second dewatering unit 30 shown in FIG.

Hereinafter, embodiments according to the present invention will be described.

6 is a graph showing the distribution of the condensation rate in the cryotrap according to the present embodiment.

The specification of the cryotrap 30 having the orifice plate 33 in the present embodiment is as follows.

Diameter r0: φ400mm

Thickness: 2mm

Material: SUS316L

Pressure P1: 1 Pa (-100 DEG C)

Pressure P2: 10-3 Pa (-100 DEG C)

Mechanism of mechanical refrigerator 18c: G-M (Gifford-McMahon) refrigerator using He

Change in pressure in the case 31: Within 30 minutes (-100 DEG C) from atmospheric pressure to 13 Pa

The pressure in the drying chamber 11 at the time of switching to the cryo trap 38 is about 1 Pa

The value of the distance d (inter-surface distance) between the orifice plate 33 and the low temperature panel 38a: 100 mm

The diameter of the opening 34 in the center portion 33c having the radius r1: 20 mm

Diameter of the opening 34 in the peripheral edge portion 33r from the radius r1 to the radius r2: 20 to 40 mm

The contour shape of the opening 34:

In this cryotrap 38, the diameter dimension of the opening 34 is changed in accordance with the radial direction (radial position) of the orifice plate 33 to adjust the diameter of the low temperature panel 38a relative to the conductance of the orifice plate 33 The condensation rate at each place was measured in the area Ra, the area rB, the area rC and the area rD shown in Fig.

Here, the condensation rate means a value obtained by dividing the number of gas molecules entering each site by the area of each site when the adsorption rate is 1.

<Experimental Example 1>

An orifice plate having a diameter of 20 mm in the center of the opening 34 in the center portion 33c, a diameter of 40 mm in the diameter of the opening 34 in the peripheral edge portion 33r, 0.8 in the center portion 33c and an aperture ratio of 0.813 in the peripheral portion 33r Experimental Example 1 was carried out.

<Experimental Example 2>

Experimental Example 2 was an orifice plate in which the diameter of the opening 34 of the center portion 33c and the peripheral portion 33r was set to 20 mm, the opening ratio of the center portion 33c was set to 0.8, and the opening ratio of the peripheral portion 33r was set to 0.765.

The results of Experimental Example 1 and Experimental Example 2 are shown in Fig.

Here, the diameters of the region rA, the region rB, the region rC, and the region rD shown in Fig. 4 are φ100 mm, φ200 mm, φ300 mm, and φ400 mm, respectively.

In Fig. 6, the condensation ratios in the regions rA to rD are normalized by setting the condensation ratio of the region rA to 1.

From this result, it can be seen that the distribution of the condensation rate of the low-temperature panel 38a in Experimental Example 1 is substantially uniform, and the condensation rate of the center in all the in-plane areas is maintained at 0.8 or more. In Experiment 2, as compared with Experimental Example 1, the condensation ratio in the region D was 0.57, indicating that the uniformity was impaired. Also in the experimental example in which the opening ratio of the peripheral edge portion 33r of Experimental Example 1 was 0.8, the distribution of the condensation rate of the low temperature panel 38a could be improved.

&Lt; Industrial applicability >

Examples of applications of the present invention include application to freeze drying, reduction of moisture content in biopharmaceuticals or antibody drugs, preservation of microorganisms (bacteria, viruses), primitive cells (protozoa, blood of mammalian cells, And application to food relations.

10 ... Vacuum drying device
11 ... drying chamber (chamber)
11a ... shelf
11b ... heater (heating means)
11c ... temperature sensor
12 ... First dehydrating part
14 ... control unit (control unit)
15 ... Vacuum pump (first exhaust means)
16 ... exhaust pump (second exhaust means)
17a ... Introduction
17b ... lead-
17c ... cooling device
19 ... washing sterilization equipment (washing sterilization unit)
21 ... first partition part
21a ... cubicle
22 ... First switching valve (first exhausting means)
23 ... second partition part
23a ... partition
24 ... second switching valve (second exhausting means)
26 ... Manometer
27 ... Manometer
F1 ... Buildings (to be degassed)
30 ... Second dehydration section (cryotrap)
31 ... case
31a ... pin
33 ... orifice plate
34 ... opening
38 ... second collecting means (cold trap)
38a ... low temperature panel
38b ... mechanical freezer

Claims (8)

A cryotrap provided with a low-temperature panel cooled by a mechanical freezer in a case connected to a chamber which is a putter space,
Wherein the plate of the low-temperature panel is disposed so as to face the object to be degassed in the chamber, and the orifice plate is disposed in front of the plate surface. The cryo trap as claimed in claim 1, wherein there is a gap between the orifice plate and the plate surface, the gap not reducing the aggregation amount on the plate surface. 3. The cryo trap as claimed in claim 1 or 2, wherein the orifice plate has a plurality of openings. 4. The cryo trap according to claim 3, wherein an opening ratio of the opening in the orifice plate is in the range of 0.8 to 0.85. 5. The cryo trap according to claim 4, wherein an opening ratio of the opening at the periphery of the orifice plate is equal to or larger than an opening ratio of the opening at the center of the orifice plate. 4. The cryo trap according to claim 3, wherein the orifice plate has a shape selected from a circle, a polygon, and a slit shape. 7. The cryo trap as claimed in claim 6, wherein the shape of the opening at the periphery of the orifice plate is the same or larger than the shape of the opening at the center of the orifice plate. The cryo-trap according to claim 1, wherein the perforator space is connected to a vacuum drying apparatus, which is a drying chamber for accommodating the laundry.

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