CN106352663A - Cryo trap - Google Patents
Cryo trap Download PDFInfo
- Publication number
- CN106352663A CN106352663A CN201610536942.0A CN201610536942A CN106352663A CN 106352663 A CN106352663 A CN 106352663A CN 201610536942 A CN201610536942 A CN 201610536942A CN 106352663 A CN106352663 A CN 106352663A
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- China
- Prior art keywords
- hothouse
- cryotrap
- trap
- orifice plate
- cold
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Classifications
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B5/00—Drying solid materials or objects by processes not involving the application of heat
- F26B5/04—Drying solid materials or objects by processes not involving the application of heat by evaporation or sublimation of moisture under reduced pressure, e.g. in a vacuum
- F26B5/06—Drying solid materials or objects by processes not involving the application of heat by evaporation or sublimation of moisture under reduced pressure, e.g. in a vacuum the process involving freezing
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61J—CONTAINERS SPECIALLY ADAPTED FOR MEDICAL OR PHARMACEUTICAL PURPOSES; DEVICES OR METHODS SPECIALLY ADAPTED FOR BRINGING PHARMACEUTICAL PRODUCTS INTO PARTICULAR PHYSICAL OR ADMINISTERING FORMS; DEVICES FOR ADMINISTERING FOOD OR MEDICINES ORALLY; BABY COMFORTERS; DEVICES FOR RECEIVING SPITTLE
- A61J3/00—Devices or methods specially adapted for bringing pharmaceutical products into particular physical or administering forms
- A61J3/02—Devices or methods specially adapted for bringing pharmaceutical products into particular physical or administering forms into the form of powders
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/14—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
- A61K9/19—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles lyophilised, i.e. freeze-dried, solutions or dispersions
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B25/00—Details of general application not covered by group F26B21/00 or F26B23/00
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B25/00—Details of general application not covered by group F26B21/00 or F26B23/00
- F26B25/06—Chambers, containers, or receptacles
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B2200/00—Drying processes and machines for solid materials characterised by the specific requirements of the drying good
- F26B2200/08—Granular materials
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- Engineering & Computer Science (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Pharmacology & Pharmacy (AREA)
- Chemical & Material Sciences (AREA)
- Medicinal Chemistry (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Molecular Biology (AREA)
- Bioinformatics & Cheminformatics (AREA)
- Epidemiology (AREA)
- Drying Of Solid Materials (AREA)
- Compressors, Vaccum Pumps And Other Relevant Systems (AREA)
Abstract
A cryo trap of the present invention is provided in a box body chamber with a degassing space, and a low temperature plate cooled by a mechanical refrigerator is spaced from the wall of the box body, wherein the plate surface of the low temperature plate is arranged to face a degassing object in the chamber. The cryo trap has an orifice plate provided in front of the plate surface.
Description
Technical field
The present invention relates to a kind of cryotrap, more particularly, it relates to a kind of be suitable to freeze-dried technology.
Background technology
Propose a kind of Minton dryer (for example, patent documentation 1) possessing cold-trap, described cold-trap passes through medicine
The material liquids such as product, food, cosmetics or chemicals freeze and are vacuum dried.
According to existing Minton dryer, it is connected with via exhaust pathway in the hothouse for housing dried object
Vacuum pump, is provided with cold-trap in the midway of this exhaust pathway.Make the water distilling out from the dried object that interior is dried by cold-trap
Devaporation and trap vapor, thus enable that dried object be dried.
In addition, as the recent trend of the freeze-dried device towards pharmaceuticals, to " antibody medicine " or " biological medicine "
Demand gradually step up.
Because the water activity that the water activity of these medicaments is higher than existing chemical substance contains it is therefore necessary to be made into
Water rate is lower.Therefore, in non-patent literature 1, by vacuum freezing drying machine will be attached to using the heat exchanger of liquid nitrogen
In making low temperature state so that reduced pressure in freeze-dried groove realize the manufacture of medicament.
In addition, manufacturing medicament in the case of these medicaments it is desirable in the case of the preparation method not changing clinical trial medicine.
But, in the technology shown in non-patent literature 1, because leading to unit scale very big using liquid nitrogen, therefore
Require equipment miniaturization, space saving.In addition, because leading to maintenance time and operating cost to increase using liquid nitrogen, therefore
Requirement need not consume this cost the excellent device and method of operability.
Therefore, it is discussed below technology (patent documentation 2): will be in quasiconductor or flat faced display (fpd, flat all the time
Panel display) manufacture device used in cryotrap be used for medicament manufacture.
Patent documentation 1: No. 5574318 publications of Japanese Patent No.
Patent documentation 2: Japanese Unexamined Patent Publication 05-044642 publication
Non-patent literature 1: positive greatly day acid skill reports gloomy public the, rice barn of no.33 (2014) p1-p2 just great " towards biological medicine
The liquid nitrogen formula vacuum freezing drying machine of product " the Internet (url；Https: //www.tn-sanso-giho.com/pdf/33/
tnscgiho33_06.pdf)
But, cryotrap is originally used for device used in quasiconductor or fpd manufacture, in manufacturing with quasiconductor or fpd
Pressure limit compare, pharmaceuticals manufacture in envision pressure limit difference double figures.Therefore, it is impossible to by this cryotrap
Directly apply to towards in the device of pharmaceuticals.
In addition, the pressure limit in pharmaceuticals manufacture is higher compared with the pressure envisioned in manufacturing in quasiconductor or fpd
Pressure limit.When therefore, in cryotrap is applied to towards the device of pharmaceuticals, as the water quantities trapping object relatively
Many.If directly applying to existing cryotrap towards in the device of pharmaceuticals, existing and cannot give full play to low temperature cold
The problem of the agglutinability of trap.
In addition, for the temperature range envisioned in manufacturing in quasiconductor or fpd, pharmaceuticals manufacture in temperature range not yet
With.Therefore, it is impossible to this cryotrap is directly applied to towards in the device of pharmaceuticals.
Content of the invention
The present invention is to propose in view of the foregoing, its be intended to reach cryotrap can be applied to freeze-dried (true
Empty it is dried) purpose in device.
The cryotrap of one mode of the present invention in the casing being connected with as the chamber being degassed space, by mechanical type
The cryopanel of fridge cooling is arranged to separate with box body wall, and wherein, the plate face of described cryopanel is provided towards described chamber
Indoor degassing object, described cryotrap possesses the orifice plate in the front being arranged at described plate face.
Thus, the pressure that may be set to the space of the space of chamber side and cryopanel side with respect to orifice plate is in prescribed limit
Interior.Even if within the temperature range of -40 DEG C～-100 DEG C about, hydrone or carbon dioxide molecule etc. also can be made in cryopanel
Coagulation constant, can stably carry out this coagulation.
Specifically, p1 will be set to closer to the pressure in the space of chamber side compared with orifice plate, will be compared with orifice plate
Closer to the pressure in the space of cryopanel side be set to p2 when, meet the critical pressure ratio of following condition by setting, Neng Goushi
Existing constant exhaust velocity.
p2/p1≤0.1
Additionally, the relation of wherein pressure p 2 and pressure p 1 meets following condition:
P1 ＞ p2.
Being provided with the cryotrap of a mode of the present invention it is also possible between described orifice plate and described plate face will not
Make the interval that the coagulation amount in described plate face declines.
The coagulation amount setting as initial condition thereby, it is possible to coagulation.
The cryotrap of one mode of the present invention can also have the multiple openings being arranged at described orifice plate.So, by
In multiple openings are provided with orifice plate, therefore only the orifice conductance according to the opening being arranged at orifice plate considering agglutinator pair
The amount of incident of low temperature plate face.Therefore, it is possible to realize above-mentioned critical pressure ratio, can make to be existed by agglutinator on the whole face of cryopanel
Equably coagulation in face.
In the cryotrap of a mode of the present invention, aperture opening ratio in described orifice plate for the described opening can also be 0.8
In the range of～0.85.
Thereby, it is possible to make to stablize as the coagulation amount that initial condition sets, can make equal in the face of cryopanel by agglutinator
The coagulation of even ground.
In the cryotrap of a mode of the present invention, aperture opening ratio in the periphery of described orifice plate for the described opening also may be used
With the aperture opening ratio in the central part of described orifice plate equal to or more than described opening.
Thereby, it is possible to the equably coagulation in face by agglutinator is made on the whole face of cryopanel.
In the cryotrap of a mode of the present invention, shape in described orifice plate for the described opening can also be selected from circle
Shape in shape shape, polygonal shape and slit-shaped.
Thereby, it is possible to realize above-mentioned critical pressure ratio.
In the cryotrap of a mode of the present invention, shape in the periphery of described orifice plate for the described opening can also
Equal to or more than shape in the central part of described orifice plate for the described opening.
Thereby, it is possible to the equably coagulation in face by agglutinator is made on the whole face of cryopanel.
In the cryotrap of a mode of the present invention, described be degassed space can also with as housing dried object
The Minton dryer of hothouse connects.
Reduce moisture content in Minton dryer for the dried object thereby, it is possible to abundant.
In accordance with the invention it is possible to realize following effect: cryotrap can be used in vacuum drying, can fully reduce
Moisture content in vacuum drying for the dried object.
Brief description
Fig. 1 is the schematic diagram of the Minton dryer representing the cryotrap being provided with one embodiment of the present invention.
Fig. 2 is the sectional view of the cryotrap representing one embodiment of the present invention.
Fig. 3 is the front view of the orifice plate in the cryotrap represent one embodiment of the present invention.
Fig. 4 is the schematic elevational view of the orifice plate in the cryotrap represent one embodiment of the present invention.
Fig. 5 is the flow chart of the Vacuum Drying Step representing the cryotrap using one embodiment of the present invention.
Fig. 6 is the chart of the condensing factor distribution in the cryotrap represent one embodiment of the present invention.
Specific embodiment
Below, based on accompanying drawing, the cryotrap of one embodiment of the present invention is illustrated.
Fig. 1 is the schematic diagram of the Minton dryer representing the cryotrap being provided with present embodiment, in FIG, attached
Icon note 10 is Minton dryer.
The Minton dryer 10 of present embodiment is in order to manufacture such as pharmaceuticals, pharmaceutical preparation and pharmaceuticals and medicine
Raw material of preparation etc., is vacuum dried by freezing this material liquid.Dried object f1 is pharmaceutical preparation or medicine system
Agent material.The state of dried object f1 can also be liquid condition in a reservoir by the collecting of above-mentioned raw materials liquid, and also permissible
Be make in the before processing operation using Minton dryer 10 described material liquid vacuum freezing solid state (for example, block,
Powder).In the present embodiment, dried object f1 is illustrated for the situation of pharmaceutical preparation or pharmaceutical preparation material.
As shown in figure 1, the Minton dryer 10 of present embodiment has: for house dried object hothouse 11,
The second de-watering section that the first de-watering section 12 being connected with hothouse 11 is independently connected with hothouse 11 with the first de-watering section 12
30th, the first lattice 21, the second lattice 23 and control unit 14 (control unit).
First de-watering section 12 has the first capturing device 17 (the first trapping mechanism), and described first capturing device 17 can pass through
Make the hydrogenesis trapping moisture distilling from dried object f1 and the first temperature can be cooled to.
Second de-watering section 30 has capturing device 38 (trapping mechanism), and described capturing device 38 can be cooled to less than the
The second temperature of one temperature.
First lattice 21 carrys out function as switching mechanism, can make hothouse 11 and the first de-watering section 12 selectivity
Ground connects or is disengaged from.
Identical with the first lattice 21, the second lattice 23 carrys out function as switching mechanism, can make hothouse 11
Selectively communicate with the second de-watering section 30 or be disengaged from.
Hothouse 11 is for making to carry out vacuum drying space as the raw material f1 of dried object.True in hothouse 11
Reciprocal of duty cycle can adjust in the range of such as 5～300pa.Hothouse 11 is had for supporting the support being placed with test portion f1 with multistage
Multiple shelf 11a of disk (figure is slightly).
Having heaters (thermoregulative mechanism) 11b is set in each of the multiple shelf 11a in hothouse 11.Heater
11b controlled unit (control unit) 14 controls, and can heat and can cool down the test portion f1 being placed on shelf 11a.As plus
Hot device 11b, for example, can be constructed by the mechanism making the inner loop in shelf 11a for the heating agent, and, can be by resistance such as sheathed heaters
Heating type heating etc. constructs.The design temperature in heating for the heater 11b is not particularly limited, for example, can be set to 20 DEG C.
At least any one shelf 11a is provided with temperature sensor 11c.Temperature sensor 11c detection is placed on and is added
The temperature of the test portion f1 on the shelf 3 of hot device 11b heating, and the temperature detecting is exported control unit as detection signal
In 14.Preferable temperature sensor 11c can on the upside of shelf 11a measurement temperature, and be arranged in each of multiple shelf 11a.
Hothouse 11 is connected with the first de-watering section 12 independently and the second de-watering section 30, hothouse 11 via this first
De-watering section 12 is connected with vacuum pump (first exhaust mechanism) 15 and pump (second exhaust mechanism) 16 with the second de-watering section 30.Vacuum pump
15 is to make to become the pump of specified vacuum degree in hothouse 11 by excluding the gas in hothouse 11.As vacuum pump 15, can
Using the various vacuum pump such as rotary pump and dry pump.
As be described hereinafter, it is provided with hothouse 11 in hothouse 11, the first de-watering section 12 and the second de-watering section 30
The cleaning being carried out and sterilizing and bactericidal unit 19 (cleaning and sterilizing mechanism).Cleaning and bactericidal unit 19 controlled unit 14
Control.Cleaning and bactericidal unit 19 can by be used for 122 DEG C about of sterilization process of steam or be used for matting meet rule
The accurate pure water of calibration is supplied to inside hothouse 11, the first de-watering section 12 and the second de-watering section 30.
It is provided with the piezometer 26,27 for measuring the pressure within hothouse 11 in hothouse 11.Piezometer 26 is
Do not affected and can be measured the first vacuometer of stagnation pressure by the measurement indicated value leading to because measuring the species of gas, for example,
Capacitance manometer as diagram vacuum gauge, diaphragm manometer.Piezometer 27 is can to measure the true of stagnation pressure using conduction of heat
Empty meter, and be to lead to because measuring the species of gas measure the second vacuometer that indicated value produces difference, for example, Pi Lani
Vacuometer.
In the first drying process being carried out by the first de-watering section 12 or heat drying operation, to by described first vacuometer
Measurement indicated value in the hothouses 11 of 26 measurements and the measurement indicated value in the hothouse 11 that measured by the second vacuometer 27 are entered
Row compares, and the difference of measurement indicated value is converged to the minimum time is judged as the first drying process or the end of heat drying operation
The point time.This is judged as differentiation operation described later.
That is, when the shape that the measured value being piezometer 26,27 from the detached state change of measured value of piezometer 26,27 is consistent
During state, can determine whether that the moisture within hothouse 11 is removed to the capacity limits of the first de-watering section 12, and be switched to by second
The second drying process that de-watering section 30 is carried out.The measured value of piezometer 26,27 is output in control unit 14.
First de-watering section 12 is as being used for aerofluxuss making hothouse 11 connect with vacuum pump (first exhaust mechanism) 15
Function is carried out in path (first exhaust path).It is provided with the first cold-trap 17 in the first de-watering section 12.First cold-trap 17 constructs
The collection face (the first collection face) of vapor can be trapped by making steam coagulation.Compared with the second cold-trap 38 described later, the
The for example, large-scale cold-trap of one cold-trap 17, is used with cold-trap as the trunk that can trap more substantial vapor is dry.
The first cold-trap 17 in first de-watering section 12 is configured to spirally wind for the pipe of cooling flow of media.As
Structure in addition, the first cold-trap 17 can also be configured to flat board (plate) shape.First cold-trap 17 has cold at the two ends of pipe
Introduction part 17a of matchmaker and leading-out portion 17b.Introduction part 17a of these coolant and leading-out portion 17b are connected with the first cooling unit 17c,
Described first cooling unit 17c supplies coolant into the first cold-trap 17 and so that it is circulated.
First cooling unit 17c controlled unit 14 controls, so that coolant circulates in the first cold-trap 17.First cooling
Unit 17c has compressor for compression refrigerant, the condensed device that the High Temperature High Pressure coolant after compression is liquefied, is used for making
The expansion valve of liquid coolant adiabatic expansion and the vaporizer that liquid coolant is gasified.First cold-trap 17 is equivalent to above-mentioned evaporation
Device.Coolant imports in the first cold-trap 17 from introduction part 17a, and derives from leading-out portion 17b after circulation in the first cold-trap 17, by
This coolant is circulated.Additionally, as coolant, such as freon r404a, silicone oil etc. can be used.
The surface (the first collection face) of the first cold-trap 17 is cooled to the first temperature by the first cooling unit 17c.First temperature
Refer to that the first cold-trap 17 can trap water and steam by making most of steam coagulation that the test portion f1 in hothouse 11 distils out
The temperature of gas.First temperature value sets according to pressure being reached as the species of the test portion f1 that object is dried, hothouse etc.
Fixed, in the present embodiment, the first temperature value is in the range of -40 DEG C about, -20 DEG C～-60 DEG C about.
For the first de-watering section 12, it is provided with to play work(as switching valve between hothouse 11 and the first cold-trap 17
First lattice 21 of energy, is provided with as switching mechanism between the first cold-trap 17 and vacuum pump (first exhaust mechanism) 15
First switching valve 22.The opening and closing controlled unit 14 of the first lattice 21 and the first switching valve 22 controls.
First lattice 21 has: spacer body 21a, can be enclosed in the part of the wall upper shed of hothouse 11；Do not scheme
The drive division showing, is used for making spacer body 21a move；With driving source (not shown), for being driven to this drive division.Drive division
The open state that the closed state that spacer body 21a is contacted with wall and spacer body 21a depart from from wall switches over.Driving source
Driving controlled unit 14 control, thus carry out the open and close controlling of the first lattice 21.As described later, spacer body 21a and drive
Dynamic portion is set to the structure being carried out when the first de-watering section 12 and hothouse 11 are carried out and are sterilized.
By open first lattice 21, hothouse 11 and the first de-watering section 12 can be made to communicate with each other.By opening simultaneously
First lattice 21 and the first switching valve 22, can make hothouse 11 and vacuum pump 15 communicate with each other.By closing the first lattice
21 and open first switching valve 22, the gas in the first de-watering section 12 can be excluded.By closing the first lattice 21 and simultaneously
One switching valve 22, can limit the gas exclusion in the hothouse 11 carrying out via the first de-watering section 12.Vacuum pump 15 and first is cut
Change valve 22 construction first exhaust mechanism.
In the present embodiment, to send out as another exhaust pathway (second exhaust path) connecting with hothouse 11
It is provided with the second cold-trap 38 in the second de-watering section 30 waving function.Second cold-trap 38 construction can be trapped by making steam coagulation
The collection face (the second collection face) of vapor.Second cold-trap 38 is configured to be cooled to and first in the first cold-trap 17
Collection face compares lower second temperature.
Fig. 2 is the sectional view of the cryotrap representing present embodiment, and Fig. 3 is the cryotrap representing present embodiment
The front view of orifice plate, Fig. 4 is the schematic elevational view of the orifice plate of the cryotrap representing present embodiment.
The cryotrap of present embodiment is arranged at vacuum and does as the second de-watering section 30 being dried for polish
Dry device 10, and be connected with as the hothouse (chamber) 11 being degassed space.
In the present embodiment, the ability fridge 17c of the first cold-trap 17 being required is as follows: realizes -50 DEG C～-60
Temperature adjustment near DEG C, and there is larger thermal capacity.On the other hand, the second cold-trap 38 is used for redrying, and is
The trap of the process after carrying out by primary drying adsorption moisture.Accordingly, as the ability that the second cold-trap 38 is required it is desirable to realize more
The temperature adjustment of low temperature (such as -80 DEG C～-100 DEG C), but thermal capacity can also be less.Therefore, compared with the first cold-trap 17, the
Two cold-traps 38 are smaller trap.Compared with the first cold-trap 17, can be less amount by the steam vapour amount that the second cold-trap 38 traps.The
Two cold-traps 38 are used as polish drying cold-trap.For example, in dried object containing 500kg about moisture in the case of,
First cold-trap 17 makes the most of moisture in dried object be dried, in order that remaining 1% moisture drying in dried object and
Using the second cold-trap 38.
Second cold-trap 38 controlled unit 14 controls, and possesses by the cryopanel 38a of mechanical type fridge 38b cooling.Low temperature
Plate 38a carrys out function as cryotrap.
As shown in Figure 2 and Figure 3, in the casing 31 of construction the second de-watering section 30, it is provided with cold by mechanical type fridge 38b
The cryopanel 38a freezing.By in the second de-watering section 30 by condensing to hydrone or carbon dioxide molecule etc. the 38a to cryopanel,
Thus maintaining these molecules etc. in the second de-watering section 30.That is, the second cold-trap 38 is configured to make the moisture within hothouse 11
Son or carbon dioxide molecule etc. reduce.
Cryopanel 38a is configured in the second dehydration in the way of separating using the casing 31 with the wall as the second de-watering section 30
In portion 30.The plate face of cryopanel 38a is disposed towards degassing object (dried object) f1 in hothouse 11 (chamber).Low
(dried object f1 side) setting abacus 33 in front of the plate face of warm plate 38a.In other words, orifice plate 33 is with positioned at hothouse 11 and low temperature
Mode between plate 38a is configured in the second de-watering section 30.
When being observed towards the direction of orifice plate 33 by dried object f1, orifice plate 33 is configured to cover the whole of cryopanel 38a
Face.Specifically, can be by providing holes in the way of the opening entirety almost covering hothouse 11 side positioned at cylindric casing 31
Plate 33.Now, orifice plate 33 is configured to not contact with casing 31, for example, pass through to be arranged to inside from casing 31 at four positions
Side project pin 31a and fix.
Orifice plate 33 is set to will not make by low temperature with the distance between cryopanel 38a d (the distance between surface, interval)
The interval that the coagulation amount of the hydrone of plate 38a coagulation or carbon dioxide molecule etc. declines.
Specifically, within being set to the mean free path to pressure p 2 for the hydrone apart from d, this pressure p 2 is and hole
Plate 33 is compared closer to the pressure in the space of cryopanel 38a side.For example, with above-mentioned coagulation amount it is necessary seizure water quantities pair
Ying Di, by cryopanel 38a have can trap this necessary catch water quantities ability in the way of setpoint distance d.
Specifically, the temperature near cryopanel 38a is -100 DEG C about and pressure is 1～10-3The device work of pa
In the case of condition, can will be set as 1～100mm apart from d.
As shown in Figure 2 and Figure 3, multiple openings 34 are provided with orifice plate 33.
The average open rate in the whole face of orifice plate 33 for this opening 34 is set to 0.8～0.85 scope.
In addition, as shown in figure 4, the configuration with regard to opening 34 and aperture opening ratio, to as having radius r1's in orifice plate 33
The central part 33c in region and as in orifice plate 33 from radius r1 to the periphery 33r in the region of radius r2 for, opening 34
Aperture opening ratio is different.Specifically, can be with the aperture opening ratio in periphery 33r equal to or more than the aperture opening ratio in central part 33c
Mode, sets the aperture opening ratio of the opening 34 of orifice plate 33.Thereby, it is possible to by hydrone or carbon dioxide molecule etc. in cryopanel 38a
Plate face in coagulation amount be set as in the face of cryopanel 38a uniformly.Therefore, it is possible at the side of cryopanel 38a or the back side
Side makes the coagulation effectively such as hydrone or carbon dioxide molecule, can effectively carry out this coagulation.
As shown in figure 3, contour shape in orifice plate 33 for the opening 34 can be round-shaped but it is also possible to be selected from polygon
Shape in shape shape, slit-shaped and mesh-shape.
In addition, as shown in figure 4, configuration as opening 34, may be set to shape in periphery 33r for the opening 34 and be equal to
Or it is more than shape in central part 33c for the opening 34.Now, shape in central part 33c for the opening 34 and opening 34 are in periphery
Shape in portion 33r can also be similar.
That is, for example, in the case that the contour shape of opening 34 is circle, may be set to opening 34 in periphery 33r
Diameter dimension is equal to or more than diameter dimension in central part 33c for the opening 34.
Thus, the coagulation in the plate face of cryopanel 38a such as hydrone or carbon dioxide molecule can be set in low temperature
On direction in the face of plate 38a uniformly.Therefore, it is possible to make hydrone or carbon dioxide divide in the side of cryopanel 38a or rear side
The coagulations effectively such as son, can carry out this coagulation effectively.
With regard to shape in orifice plate 33 for the opening 34 or configuration etc., will be closer to hothouse (chamber) compared with orifice plate 33
Pressure in the space of 11 sides is set to p1, will be set to p2 closer to the pressure in the space of cryopanel 38a side compared with orifice plate 33
When, the critical pressure ratio meeting following condition can be set.
p2/p1≤0.1
Thereby, it is possible to realize constant exhaust velocity.Additionally, wherein pressure p 2 and the relation of pressure p 1 meet following bar
Part:
P1 ＞ p2.
Cryopanel 38a can make helium carry out simon (simon) expansion by mechanical type fridge 38b and be cooled to for example
The ultralow temperature of 80k.By gas molecule condensing on cryopanel 38a, the vacuum in hothouse 11 can be improved to exhaust pump
16 etc. are beyond one's reach fine vacuum.
Exhaust pump 16 has to the function of carrying out vacuum exhaust in the second de-watering section 30, can use turbine as exhaust pump 16
Molecular pump.
The surface (the second collection face) of cryopanel 38a is cooled to the surface temperature less than the first cold-trap 17 by the second cold-trap 38
, e.g., from about -70 DEG C～-100 DEG C, -85 DEG C about.If being set as the surface temperature of cryopanel 38a too low, necessary
The ability of mechanical type fridge 38b is excessive, therefore not preferred.In addition, if the surface temperature of cryopanel 38a was set as
Height, then cannot be reduced to desired level by the moisture content of dried object f1, therefore not preferred.
Additionally, as described above, the second cold-trap 38 script is cold using the high performance low temperature that can be applicable to quasiconductor or fpd manufacture
Trap, but the second cold-trap 38 can also be used under conditions of extremely different from the condition being usually used.
For the second de-watering section 30, it is provided with to play work(as switching valve between hothouse 11 and the second cold-trap 38
Second lattice 23 of energy.It is provided with as switching mechanism between the second cold-trap 38 and exhaust pump (second exhaust mechanism) 16
Second switching valve 24.The opening and closing controlled unit 14 of the second lattice 23 and the second switching valve 24 controls.
Second lattice 23 has: spacer body 23a, can be enclosed in the part of the wall upper shed of hothouse 11；Do not scheme
The drive division showing, is used for making spacer body 23a move；With driving source (not shown), for being driven to this drive division.Drive division
The open state that the closed state that spacer body 23a is contacted with wall and spacer body 23a depart from from wall switches over.Driving source
Driving controlled unit 14 control, thus carry out the open and close controlling of the second lattice 23.As described later, spacer body 23a and drive
Dynamic portion is set to the structure being carried out when the second de-watering section 30 and hothouse 11 are carried out and are sterilized.
Spacer body 23a is configured in the position compared with orifice plate 33 closer to dried object f1 in hothouse 11.
By open second lattice 23, hothouse 11 and the second de-watering section 30 can be made to communicate with each other.By opening simultaneously
Second lattice 23 and the second switching valve 24, can make hothouse 11 and exhaust pump (second exhaust mechanism) 16 communicate with each other.Pass through
Close the second lattice 23 open second switching valve 24, the gas in the second de-watering section 30 can be excluded.By closing simultaneously
Two compartment portion 23 and the second switching valve 24, can be in autonomous closure the second de-watering section 30 and hothouse 11.Exhaust pump 16 and second is cut
Change valve 24 construction second exhaust mechanism.
The Minton dryer 10 of present embodiment is being carried out to hothouse 11, the first de-watering section 12 and the second de-watering section 30
After cleaning, while connection hothouse 11 and the first de-watering section 12, close the second de-watering section 30, thus carry out first to freeze to do
Drying process.Afterwards, while connecting hothouse 11 and the second de-watering section 30, close the first de-watering section 12, thus carrying out the second jelly
Knot drying process.
Therefore, in the Minton dryer 10 of present embodiment, hothouse 11, the first de-watering section 12 and the second de-watering section
30 are able to be cleaned by and can be airtight.
Specifically, for the first de-watering section 12 and the second de-watering section 30, as hot countermeasure during sterilizing, pharmaceutical preparation
Manufacture countermeasure, can set spacer body 21a, the drive division of spacer body 21a, spacer body 23a, the drive division of spacer body 23a and low
The surface of warm plate 38a (cryotrap) is by plated structure such as sus, sus316, au, pt.Additionally, the surface not being cleaned by
The part not connected with the inner surface of de-watering section 12,30 can also be using the good cu of electric heating.
First switching valve 22 and compared with the first switching valve 22 closer to vacuum pump 15 side for gas will not from first dehydration
Portion 12 is to the structure of hothouse 11 adverse current.Equally, the second switching valve 24 and compared with the second switching valve 24 closer to exhaust pump 16
Side will not be from the second de-watering section 30 to the structure of hothouse 11 adverse current for gas.
With regard to cryotrap, clip in generally for the connecting portion raising conductivity of heat to fridge and trap plate in this part
Paper tinsel is but it is also possible to be changed to gold-plated, native gold etc. by this in paper tinsel from paper tinsel.
In addition, in the second de-watering section 30, for the vacuum drying method of present embodiment described later, in sterilizing work
In sequence, matting, collecting operation, the first drying process, closer to row compared with the second switching valve 24 of second exhaust mechanism
Air pump 16 side is the state of closing.
Below, the vacuum drying method of the cryotrap using present embodiment is illustrated.
Fig. 5 is the flow chart of the vacuum drying method representing the cryotrap using present embodiment.
As shown in figure 5, there is preparatory process s01, opening and closing using the vacuum drying method of the cryotrap of present embodiment
Operation s02, sterilization process s03, matting s04, predry drying process s05, opening and closing operation s06, collecting operation s07, opening and closing work
Sequence s08, the first drying process s09, heat drying operation s10, second exhaust operation s11, differentiation operation s12, opening and closing operation
S13, the second drying process s14, first exhaust operation s15, airtight operation s16, opening and closing operation s17 and removal process s18.
With regard to the vacuum drying method of present embodiment, as the preparatory process s01 shown in Fig. 5, preparing in advance into can
Necessary dried object f1 is moved on shelf 11a.In addition, control unit 14 prepares necessary manufacturing condition information.
Then, as opening and closing operation s02 shown in Fig. 5, by the control of control unit 14, it is opened and closed each point as follows
Every portion and valve.
Hothouse 11: open
First lattice 21: open
Second lattice 23: open
First switching valve 22: close
Second switching valve 24: close
Then, as the sterilization process s03 shown in Fig. 5, in the state of being set by opening and closing operation s02, that is, open the
One lattice 21 with the second lattice 23 so that in the state of hothouse 11, the first de-watering section 12 connect with the second de-watering section 30,
By the control of control unit 14, from the mechanism 19 supply steam that cleans and sterilize.Thus, to hothouse 11, the first de-watering section 12
Sterilized with the inside of the second de-watering section 30.
The part that exposed for the pharmaceutical preparation as dried object f1 is it is necessary to ensure that integral asepsis.Therefore, Mei Dangkai
During beginning medicament production process, as the front operation of medicament production process, carry out steam sterilization operation s03.Jelly towards pharmaceuticals
Sterilizing required for knot drying device refers to by exposing more than 20 minutes and eliminating bacteria in the steam more than 122 DEG C.
Pressure in this steam sterilization operation be 210kpa about, 220kpa～240kpa.In fact, as steam
Sterilization process s03, will maintain three hours about at high temperature inside device.
Now, in order to tolerate this temperature, the pipe for cooling flow of media of the first cold-trap 17 is configured to by making cooling
Unit 17c drives operating to keep less than 70 DEG C.
Equally, in order to tolerate this temperature, the cryopanel 38a of the second cold-trap 38 is configured in heating by making mechanical type
Fridge 38b drives and operates and less than 70 DEG C of mechanical type fridge 38b holding.In the past, when the cryotrap being used is arrived
From during the heat transfer of cryopanel 38a, the heat resisting temperature of mechanical type fridge 38b is 70 DEG C, and thus described cryotrap is maintained at machine
Below the heat resisting temperature of tool formula fridge 38b.In addition, also improving the thermostability of mechanical type fridge 38b.
Then, as matting s04 shown in Fig. 5, in the state of being set by opening and closing operation s02, that is, open the
One lattice 21 with the second lattice 23 so that in the state of hothouse 11, the first de-watering section 12 connect with the second de-watering section 30,
By the control of control unit 14, supply the pure water for cleaning and meeting required standard from cleaning and sterilizing mechanism 19.Thus,
The inside of hothouse 11, the first de-watering section 12 and the second de-watering section 30 is carried out.With other manufacture fields such as quasiconductors
Vacuum equipment is different, to be cleaned by watering to the inside of device.It is therefore preferable that hothouse 11, the first de-watering section 12 and second are de-
The inside in water portion 30 is the structure as far as possible not accumulating water.
Then, as the predry drying process s05 shown in Fig. 5, in the state of being set by opening and closing operation s02, that is, opening
First lattice 21 is with the second lattice 23 so that the state that connects with the second de-watering section 30 of hothouse 11, the first de-watering section 12
Under, the first cold-trap 17 is driven by the control of control unit 14, with to hothouse 11, the first de-watering section 12 and the second de-watering section
30 carry out predrying, thus removing rinse water.Now, the register (thermoregulative mechanism) of shelf 11a can be passed through, to hothouse 11
Inside heated.
In predry drying process s05, control unit 14 makes coolant in the first cold-trap by driving the first cooling unit 17c
Circulate in 17, and open the first lattice 21, the second lattice 23 and the first switching valve 22 and close the second switching valve 24, lead to
Overdrive vacuum pump 15 and exclude the gas in hothouse 11 via the first de-watering section 12 as first exhaust path.Thus,
The moisture evaporation of inside because of the pressure drop of hothouse 11, the first de-watering section 12 and the second de-watering section 30.Vacuum pump 15 via
The gas of the inside of the hothouse 11 containing vapor, the first de-watering section 12 and the second de-watering section 30 is aspirated in first exhaust path.
Vapor is trapped by the first cold-trap 17.
Additionally, in predry drying process s05, preferably do not drive the second cold-trap 38, but because of second exhaust operation described later
S11 and exclude in subsequent handling in situation of moisture within the second de-watering section 30 etc. however it is not limited to this.
Then, as opening and closing operation s06 shown in Fig. 5, by the control of control unit 14, it is opened and closed each point as follows
Every portion and valve.
Hothouse 11: open
First lattice 21: open
Second lattice 23: close
First switching valve 22: close
Second switching valve 24: close
Then, as collecting operation s07 shown in Fig. 5, in the state of being set by opening and closing operation s06, that is, open the
So that while hothouse 11 connects with the first de-watering section 12, closing the second lattice 23 is so that the second de-watering section for one lattice 21
In the state of 30 independences, dried object f1 is moved in hothouse 11.
Then, as opening and closing operation s08 shown in Fig. 5, by the control of control unit 14, it is opened and closed each point as follows
Every portion and valve.
Hothouse 11: close
First lattice 21: open
Second lattice 23: close
First switching valve 22: open
Second switching valve 24: close
Then, as the first drying process s09 shown in Fig. 5, in the state of being set by opening and closing operation s08, that is, opening
Put the first lattice 21 so that while hothouse 11 connects with the first de-watering section 12, closing the second lattice 23 is so that second is de-
In the state of water portion 30 independence, the first cold-trap 17 is driven by the control of control unit 14, with de- to hothouse 11 and first
The inside in water portion 12 particularly hothouse 11 carries out freeze-dried.Thus, because under the pressure of hothouse 11 and the first de-watering section 12
Drop and the moisture evaporation of inside.Vacuum pump 15 aspirates the gas in the hothouse 11 containing vapor via first exhaust path.
Vapor is trapped by the first cold-trap 17.
The non-condensing gases such as the nitrogen from the gas of hothouse 11 suction are aspirated without in the first cold-trap by vacuum pump 15
Condense in 17.Freeze the test portion f1 being placed on shelf 11a by depriving evaporation latent heat from moisture.
The temperature of the first cold-trap 17 in the first drying process s09 is set to -40 DEG C about.
Then, as heat drying operation s10 shown in Fig. 5, in the state of being set by opening and closing operation s08, that is, opening
Put the first lattice 21 so that while hothouse 11 connects with the first de-watering section 12, closing the second lattice 23 is so that second is de-
In the state of water portion 30 independence, the register 11b being arranged at each shelf 11a is driven by the control of control unit 14
(thermoregulative mechanism).
Heater (thermoregulative mechanism) 11b by the shelf 11a in hothouse 11 is heated to 20 DEG C and to being placed on shelf
Test portion f1 on 11a is heated, and thus promotes the drying of test portion f1.In heated test portion f1, contained ice is from this test portion
Obtain latent heat in f1, and vapor is become by distillation.
Vacuum pump 15 aspirates the gas in the hothouse 11 containing this vapor via first exhaust path.By vacuum pump 15
Vapor in the gas of suction discharges latent heat on the surface of the first cold-trap 17, and becomes ice by condensing, by this vapor
Trapped by the first cold-trap 17.The non-condensing gas such as nitrogen from the gas of hothouse 11 suction by vacuum pump 15 aspirate without
Condense in first cold-trap 17.
By proceeding the bleeding of the hothouse 11 being carried out by vacuum pump 15, thus hothouse 11 reaches vacuum pump
15 have reach pressure.In addition, because set point in hothouse 11 for the vapor declines and the trapping energy of the first cold-trap 17
Power is deteriorated, thus the vacuum in hothouse 11 rises stopping.If the vacuum in hothouse 11 rises stopped, test portion f1
In contained ice cannot distil.As a result, because contained ice in test portion f1 in the case of not distilled will not be from
Latent heat is obtained, the temperature of test portion f1 rises therefore by the heat effect of heater 11b in solid material.It is arranged on shelf
The surface temperature of the test portion f1 that the temperature sensor 11c detection on 11a is heated by heater 11b, and the temperature detecting is made
Export in control unit 14 for detection signal.
Meanwhile, by proceeding the bleeding of hothouse 11 being carried out by vacuum pump 15, thus in hothouse 11
Vacuum rises and stops.Now, the measurement indicated value of the measurement indicated value of piezometer 26 and piezometer 27 is exported control single
In unit 14, wherein, described piezometer 26 is can not surveyed by affect by the measurement indicated value that the species of measurement gas causes
First vacuometer of amount stagnation pressure, described piezometer 27 is can measure the vacuometer of stagnation pressure and be because measuring gas using conduction of heat
The species of body and measure indicated value produce difference the second vacuometer.
Control unit 14 is to the measurement indicated value in the hothouse 11 being measured by described first vacuometer 26 and true by second
Measurement indicated value in the hothouses 11 of empty meter 27 measurement is compared, and when detecting that the difference of measurement indicated value converges to minimum
Between.By being compared to the difference of the measurement indicated value in these first vacuometers and the second vacuometer, by this measurement indicated value
Difference converge to the minimum time and be judged as terminal acknowledging time is dried, thus under the second vacuometer is measured in indicative curve
Fall point of inflexion on a curve time detecting is that terminal acknowledging time is dried.
Meanwhile, control unit 14, based on the detection signal from temperature sensor 11c, detects the surface temperature of test portion f1
Equal with the heating-up temperature of heater 11b and reach the upper limit.
Then, as differentiation operation s12 shown in Fig. 5, be judged as reaching terminal acknowledging time and/or the upper limit are dried when
Between in the case of, control unit 14 is judged as the terminal time that this time is heat drying operation s10, wherein, described dry eventually
Point acknowledging time is by the measurement indicated value from piezometer 26,27 is compared with the time detecting, the described upper limit
Time is surface temperature and the heater 11b of the test portion f1 being detected based on the detection signal from temperature sensor 11c
The temperature equal time.Now, first, after closing the first lattice 21, stop the driving of the first cold-trap 17.If additionally,
Close the first lattice 21, then the open and-shut mode of the first switching valve 22 can be any state.
Then, as opening and closing operation s13 shown in Fig. 5, by the control of control unit 14, it is opened and closed each point as follows
Every portion and valve.
Hothouse 11: close
First lattice 21: close
Second lattice 23: open
First switching valve 22: close
Second switching valve 24: open
Then, as the second drying process s14 shown in Fig. 5, in the state of being set by opening and closing operation s13, that is, opening
Put the second lattice 23 so that while hothouse 11 connects with the second de-watering section 30, closing the first lattice 21 is so that first is de-
In the state of water portion 12 independence, the second cold-trap 38 is driven by the control of control unit 14, with de- to hothouse 11 and second
The inside in water portion 30 particularly hothouse 11 carries out freeze-dried.
Thus, the moisture evaporation of inside because of the pressure drop of hothouse 11 and the second de-watering section 30.Turbomolecular pump 16
Aspirate the gas in the hothouse 11 containing vapor via second exhaust path.Vapor is by the low temperature cold as the second cold-trap
Trap 38 traps.
Meanwhile, the pressure in pressure p 1 and the cryopanel 38a side space in hothouse 11 side space is realized by orifice plate 33
The pressure ratio of p2 meets
P2 (pressure of cryopanel 38a side)/p1 (pressure of hothouse 11 side)≤0.1
P1 ＞ p2
Condition critical pressure ratio, thus, it is possible to stable and constant exhaust velocity is realized by cryotrap 38.
Now, for cryopanel 38a is positioned at the surface of hothouse 11 side, water (hydrone) can be in cryopanel 38a
Face in by equably coagulation, and make ice coagulation on the surface of cryopanel 38a, with fill up orifice plate 33 and cryopanel 38a it
Between the space apart from d.Equally it is also possible to make ice in the back side coagulation of cryopanel 38a.Additionally, orifice plate 33 need not be cooled to
With cryopanel 38a identical degree, but the state after cooling also can be become.
Additionally, heater 11b and turbomolecular pump 16 are set as lasting driving condition from heat drying operation s10.Separately
Outward it is also possible to before the second lattice 23 is open, start the driving of cryotrap 38.
The temperature of cryotrap 38 is less than the temperature of the first cold-trap 17, for example, be set to -100 DEG C about.
The second cold-trap 38 being cooled to -100 DEG C traps to the vapor not trapped by the first cold-trap 17.Adjoint
This, the pressure drop of hothouse 11.Thus, restart to remain in the distillation of the ice in test portion f1.Remain in test portion f1
Ice is distilled by obtaining latent heat from test portion f1, the surface release of the vapor of the generation cryopanel 38a in the second cold-trap 38
Latent heat simultaneously condenses and becomes ice, thus being trapped by the second cold-trap 38.It is dried by this polish, heated drying process can be made
S10 dried test portion f1 is dried further, and improves the final aridity of test portion f1, so that moisture content declines two
Number.Additionally, with respect to the water removing in the first drying process s09 using the first de-watering section 12 and heat drying operation s10
Point, the moisture removing in the second drying process s14 using the second de-watering section 30 is 1% about i.e. 5kg.
Then, as airtight operation s16 shown in Fig. 5, in the state of being set by opening and closing operation s13, that is, open the
So that while hothouse 11 connects with the second de-watering section 30, closing the first lattice 21 is so that the first de-watering section in two compartment portion 23
In the state of 12 independences, by the control of control unit 14, using obturator (not shown) (closure mechanism) to dried object
It is airtight etc. airtight to carry out that f1 implements aluminum.
Then, as opening and closing operation s17 shown in Fig. 5, by the control of control unit 14, it is opened and closed each point as follows
Every portion and valve.
Hothouse 11: open
First lattice 21: close
Second lattice 23: close
First switching valve 22: close
Second switching valve 24: close
Then, as removal process s18 shown in Fig. 5, take out moisture content from hothouse 11 and be reduced to the expectation state simultaneously
Dried object f1 that dried terminates, thus terminate the dried in this batch.
Additionally, as shown in figure 5, in part or all of the first drying process s09 and heat drying operation s10, making
For second exhaust operation s11, in the state of being set by opening and closing operation s08, that is, in open first lattice 21 so that hothouse
11 while connect with the first de-watering section 12, and closing the second lattice 23 is so that in the state of the second de-watering section 30 independence, pass through
Open the second switching valve 24, exclusion becomes the gas in the second de-watering section 30 of this separate state, thus will be by the second cold-trap 38
The moisture of trapping is rejected to outside.Thereby, it is possible to immediately begin to the freeze-dried operation of next batch.
Equally, in part or all of the second drying process s14 shown in Fig. 5, as first exhaust operation s15,
In the state of being set by opening and closing operation s13, that is, in open second lattice 23 so that hothouse 11 and the second de-watering section 30 connect
While logical, closing the first lattice 21 is so that in the state of the first de-watering section 12 independence, by opening the first switching valve 22, arrange
Except the gas becoming in the first de-watering section 12 of this separate state, thus outer by being rejected to by the moisture that the first cold-trap 17 traps
Portion.Thereby, it is possible to immediately begin to the freeze-dried operation of next batch.
In the present embodiment, one of two cold-traps allowing hand over 17,38 are made to become independent cryotrap 38,
And by arranging orifice plate 33, thus dried object can be carried out freeze-dried until moisture content becomes and was beyond one's reach down in the past
Double-digit moisture content drops.
Further, since compared with being proposed to obtain the method for lower temperature by liquid nitrogen, operation cost is cheap in the past
And temperature conditionss can also be changed, therefore, it is possible to tackle various drying conditions.
When starting cryotrap 38, become closed state by making the first lattice 21 or the second lattice 23, thus
Can prevent the ice being attached to the first cold-trap 17 from adsorbing on the lower cryotrap for the treatment of temperature 38 compared with the first cold-trap 17
Probability.
In addition it is also possible to install the other separations in addition to the second lattice 23 between cryotrap 38 and hothouse 11
Valve is not so that destroy the function of orifice plate 33.
Or it is also possible to according to the species of dried object f1 or the restriction that leads to because of dried object f1, maintenance can be tieed up
Hold above-mentioned critical pressure ratio assigned position relation while, the cryopanel 38a in cryotrap 38 and orifice plate 33 are directly set
Put in hothouse 11.This structure can be applicable to following situation: such as dried object f1 is the product being removed after airtight
Situation etc. and the ice being attached to cryotrap 38 will not cause the situation of problem in product warehouse-out.
In addition, identical with the first cold-trap 17 it is also possible to existing freeze-dried device perforate additional valve, and add
Cryotrap 38.At this time, it may be necessary to being set to above-mentioned specification or being set to the structure according to this specification so that can be applicable to clean
And sterilization process.
In dried, dried object f1 expose the inside of hothouse 11, the inside of the first de-watering section 12, second take off
The inside in water portion 30 must assure that integral asepsis.Therefore, whenever starting medicament production process, before medicament production process
Operation is it is necessary to carry out steam sterilization operation and matting.Towards pharmaceuticals particularly be applied to water for injection (wfi:
Water for injection) manufacture etc. freeze-dried device in necessary sterilization treatment refer to by more than 122 DEG C
Steam in expose more than 20 minutes and eliminating bacteria.
Inside hothouse 11 pressure in this steam sterilization operation be 210kpa about, 220kpa～240kpa.
In fact, as steam sterilization operation, high temperature three hours about will be maintained inside device.Now, in the first cold-trap 17, in order to
Tolerate this temperature, keep less than 70 DEG C of temperature by making cooling unit 17c operate.In addition, in this trap of cryotrap 38
In, in order to tolerate this temperature, so that it is operated by starting the compressor of mechanical type fridge 38b when steam heats, thus protecting
Hold less than 70 DEG C of temperature.
Due in cryotrap 38, mechanical type fridge 38b cannot keep in the environment of more than 70 DEG C for a long time, because
This is preferably carried out at sterilizing while mechanical type fridge 38b being set to operating condition and cooled down in sterilization process s03
Reason.At this time, it may be necessary to carry out mechanical type fridge 38b output set so that the cooling capacity of mechanical type fridge 38b higher and
The temperature of trap plate 38a reaches the temperature enough to sterilize.
In addition, in the case of the device that such as present embodiment manufactures towards pharmaceutical preparation, as mechanical type
The connecting portion of fridge 38b and cryopanel 38a improves the paper tinsel body of heat transfer, can use gold-plated, native gold etc..
The first drying process s09 and heat drying operation s10 of water is trapped in the first cold-trap 17 at -50 DEG C～-70 DEG C
After end, carry out the second drying process s14 as total polish further, in this operation, cryotrap 38 is at -90 DEG C
Residual moisture is drawn at～-100 DEG C.It is therefore preferable that the first cold-trap 17 and cryotrap 38 are arranged on the room (space) separating.
Additionally, it is preferred that not using heater 11b for the ice-melt in cryopanel 38a.
For cryotrap 38, the material in the cylinder body portion of mechanical type fridge 38b is sus316.In addition, cryopanel (trap
Plate) material of 38a part is sus316, heat transfer part formed by the higher metal of the corrosion resistances such as native gold.
Reducing the second drying process s14 of the moisture content of dried object f1 by trapping moisture at very low temperature is
Carry out the finishing step after the first freeze-dried drying process s09, remaining some moisture of absorption under conventional operating.
Therefore, in the Minton dryer of present embodiment, its object is to when processing speed rising need not be made and shortens process
Between in the case of, the degree that reaches of moisture content is improved about double figures.In the past, select for quasiconductor or flat faced display
Cryotrap 38 in the manufacture device of (fpd, flat panel display), cryotrap 38 can be used for present embodiment
Minton dryer.
Additionally, in the present embodiment, the surface configuration by orifice plate 33 and cryopanel 38a is towards dried object f1, but
The present invention does not limit this configuration.If can be towards dried object f1 and full to be configured to orifice plate 33 and cryopanel 38a
The mode of above-mentioned critical pressure ratio p1/p2 of foot configures orifice plate 33, then the second de-watering section 30 may be connected under hothouse 11
Side, and also the position of the position of the first de-watering section 12 shown in Fig. 1 and the second de-watering section 30 can be changed.
[embodiment]
Below, embodiments of the invention are illustrated.
Additionally, illustrating to the concrete example of the present invention.
Fig. 6 is the chart of the condensing factor distribution in the cryotrap represent present embodiment.
The parameters of the cryotrap 38 with orifice plate 33 in the concrete example of present embodiment described below.
Diameter r0: φ 400mm
Thickness: 2mm
Material: sus316l
Pressure p 1:1pa (- 100 DEG C)
Pressure p 2:10-3pa(-100℃)
The mode of mechanical type fridge 18c: the g-m (gifford-mcmahon, Ji Fude-McMahon) using he is cold
Jelly machine
Pressure change in casing 31: from change of atmospheric pressure to 13pa (- 100 DEG C) within 30 minutes
Switch to the pressure in the hothouse 11 during cryotrap 38: about 1pa
The distance between orifice plate 33 and cryopanel 38a d (distance between surface) value: 100mm
Diameter in central part 33c in radius r1 for the opening 34: φ 20mm
Diameter in the periphery 33r from radius r1 to radius r2 for the opening 34: φ 20～40mm
The contour shape of opening 34: cast (circular)
For this cryotrap 38, by making diametric(al) (the radius side of the diameter dimension of opening 34 along orifice plate 33
To position) change, comes region ra as shown in Figure 4, region rb, region rc, region rd measurement with respect to the conductance of orifice plate 33
Condensing factor in cryopanel 38a each position.
Here, condensing factor refers to incide the face divided by each position for the gas molecula number in each position when adsorption rate is 1
Long-pending value.
<experimental example 1>
By using orifice plate as experimental example 1: radius in central part 33c for the opening 34 is set to φ 20mm, opening 34
Radius in periphery 33r is set to φ 40mm, and the aperture opening ratio in central part 33c is set to 0.8, in periphery 33r
Aperture opening ratio be set to 0.813.
<experimental example 2>
By using orifice plate as experimental example 2: radius in central part 33c and periphery 33r for the opening 34 is set to φ
20mm, the aperture opening ratio in central part 33c is set to 0.8, and the aperture opening ratio in periphery 33r is set to 0.765.
Fig. 6 illustrates experimental example 1, the result of experimental example 2.
Here, each diameter of the region ra shown in Fig. 4, region rb, region rc, region rd is respectively φ 100mm, φ
200mm、φ300mm、φ400mm.
In addition, in figure 6, with the condensing factor of region ra for 1, the condensing factor in each region ra～rd is normalized.
From this result, in experimental example 1, the condensing factor 38a distribution of cryopanel 38a is generally uniform, whole in face
Region, the condensing factor at center is maintained at more than 0.8.And understand, compared with experimental example 1, solidifying in region d in experimental example 2
Shrinkage is 0.57, destroys uniformity.Even if additionally, the periphery 33r by experimental example 1 aperture opening ratio be set to 0.8 experiment
It is also possible to improve the condensing factor distribution of cryopanel 38a in example.
Industrial applicability
As the application examples of the present invention, can enumerate to be directed to requiring to be suppressed to the moisture content of biological medicine and antibody medicine etc.
Relatively low freeze-dried application or be directed to microorganism (antibacterial, virus), the living cells (blood of protozoacide and cells of mamma animals
And sperm) preservation, the application of food relation.
Description of reference numerals
10 ... Minton dryers
11 ... hothouses (chamber)
11a ... shelf
11b ... heater (thermoregulative mechanism)
11c ... temperature sensor
12 ... first de-watering section
14 ... control units (control unit)
15 ... vacuum pumps (first exhaust mechanism)
16 ... exhaust pumps (second exhaust mechanism)
17 ... first trappings mechanism (the first cold-trap)
17a ... introduction part
17b ... leading-out portion
17c ... cooling unit
19 ... cleanings and bactericidal unit (cleaning and sterilizing mechanism)
21 ... first lattices
21a ... spacer body
22 ... first switching valves (first exhaust mechanism)
23 ... second lattices
23a ... spacer body
24 ... second switching valves (second exhaust mechanism)
26 ... piezometers
27 ... piezometers
F1 ... dried object (degassing object)
30 ... second de-watering section (cryotrap)
31 ... casings
31a ... sells
33 ... orifice plates
34 ... openings
38 ... second trappings mechanism (cold-trap)
38a ... cryopanel
38b ... mechanical type fridge
Claims (8)
1. a kind of cryotrap, in the casing being connected with as the chamber being degassed space, is cooled down by mechanical type fridge
Cryopanel is arranged to separate with box body wall, wherein,
The plate face of described cryopanel is disposed towards the degassing object of described within the chamber,
Described cryotrap possesses the orifice plate in the front being arranged at described plate face.
2. cryotrap according to claim 1, wherein,
It is provided with the interval that the coagulation amount in described plate face will not be made to decline between described orifice plate and described plate face.
3. cryotrap according to claim 1 and 2, wherein,
There are the multiple openings being arranged at described orifice plate.
4. cryotrap according to claim 3, wherein,
Aperture opening ratio in described orifice plate for the described opening is 0.8～0.85 scope.
5. cryotrap according to claim 4, wherein,
Aperture opening ratio in the periphery of described orifice plate for the described opening is equal to or more than the central part in described orifice plate for the described opening
In aperture opening ratio.
6. cryotrap according to claim 3, wherein,
Described opening is in the shape being shaped as in round-shaped, polygonal shape and slit-shaped in described orifice plate.
7. cryotrap according to claim 6, wherein,
Described opening is equal to or more than described opening in the central part of described orifice plate in the shape in the periphery of described orifice plate
Shape.
8. cryotrap according to claim 1, wherein,
The described space that is degassed is connected with the Minton dryer as the hothouse housing dried object.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2015-139977 | 2015-07-13 | ||
| JP2015139977A JP6639129B2 (en) | 2015-07-13 | 2015-07-13 | Cryotrap |
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| CN106352663A true CN106352663A (en) | 2017-01-25 |
| CN106352663B CN106352663B (en) | 2020-01-17 |
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| Country | Link |
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| JP (1) | JP6639129B2 (en) |
| KR (1) | KR102076299B1 (en) |
| CN (1) | CN106352663B (en) |
| TW (1) | TWI612218B (en) |
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| CN107560329A (en) * | 2017-07-27 | 2018-01-09 | 郑州联慧双创知识产权代理有限公司 | A kind of bio-feritlizer rapid freeze-drying device |
| CN116116035B (en) * | 2023-02-14 | 2023-11-14 | 湖北省智云冷锋环保科技有限公司 | Industrial low-temperature cold trap and temperature control method |
Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4896511A (en) * | 1987-01-27 | 1990-01-30 | Lessard Philip A | Optimally staged cryopump |
| JPH0544642A (en) * | 1991-08-13 | 1993-02-23 | Ulvac Kuraio Kk | Cryopump equipped with low temperature trap |
| CN101059303A (en) * | 2006-04-21 | 2007-10-24 | 北美冻干技术股份公司 | Plate type cold trap for freeze-dryer |
| JP2010084702A (en) * | 2008-10-01 | 2010-04-15 | Sumitomo Heavy Ind Ltd | Cryopump |
| CN201551867U (en) * | 2009-11-16 | 2010-08-18 | 沈阳航天新阳速冻设备制造有限公司 | Plate beam type cold trap |
| JP2010270928A (en) * | 2009-05-19 | 2010-12-02 | Ulvac Japan Ltd | Vacuum drying device and vacuum drying method |
| JP2011117464A (en) * | 2011-03-24 | 2011-06-16 | Sumitomo Heavy Ind Ltd | Cryopump |
| JP2011167647A (en) * | 2010-02-19 | 2011-09-01 | Sumitomo Heavy Ind Ltd | Cold trap and vacuum exhaust device |
| US20130312431A1 (en) * | 2011-02-09 | 2013-11-28 | Sergei Syssoev | Cryopump |
| CN104074715A (en) * | 2013-03-25 | 2014-10-01 | 住友重机械工业株式会社 | Cryopump and vacuum pumping method |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2888373Y (en) * | 2005-11-08 | 2007-04-11 | 上海东富龙科技有限公司 | Freezing-drying machine with liquid nitrogen to assist refrigerate |
-
2015
- 2015-07-13 JP JP2015139977A patent/JP6639129B2/en active Active
-
2016
- 2016-07-01 TW TW105121009A patent/TWI612218B/en active
- 2016-07-06 KR KR1020160085788A patent/KR102076299B1/en active IP Right Grant
- 2016-07-08 CN CN201610536942.0A patent/CN106352663B/en active Active
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4896511A (en) * | 1987-01-27 | 1990-01-30 | Lessard Philip A | Optimally staged cryopump |
| JPH0544642A (en) * | 1991-08-13 | 1993-02-23 | Ulvac Kuraio Kk | Cryopump equipped with low temperature trap |
| CN101059303A (en) * | 2006-04-21 | 2007-10-24 | 北美冻干技术股份公司 | Plate type cold trap for freeze-dryer |
| JP2010084702A (en) * | 2008-10-01 | 2010-04-15 | Sumitomo Heavy Ind Ltd | Cryopump |
| JP2010270928A (en) * | 2009-05-19 | 2010-12-02 | Ulvac Japan Ltd | Vacuum drying device and vacuum drying method |
| CN201551867U (en) * | 2009-11-16 | 2010-08-18 | 沈阳航天新阳速冻设备制造有限公司 | Plate beam type cold trap |
| JP2011167647A (en) * | 2010-02-19 | 2011-09-01 | Sumitomo Heavy Ind Ltd | Cold trap and vacuum exhaust device |
| US20130312431A1 (en) * | 2011-02-09 | 2013-11-28 | Sergei Syssoev | Cryopump |
| JP2011117464A (en) * | 2011-03-24 | 2011-06-16 | Sumitomo Heavy Ind Ltd | Cryopump |
| CN104074715A (en) * | 2013-03-25 | 2014-10-01 | 住友重机械工业株式会社 | Cryopump and vacuum pumping method |
Non-Patent Citations (1)
| Title |
|---|
| 蔡津生,卢国宝: "《中国食药用菌工程学（2015.1）》", 31 January 2015 * |
Also Published As
| Publication number | Publication date |
|---|---|
| TW201712224A (en) | 2017-04-01 |
| JP6639129B2 (en) | 2020-02-05 |
| TWI612218B (en) | 2018-01-21 |
| KR20170008161A (en) | 2017-01-23 |
| CN106352663B (en) | 2020-01-17 |
| KR102076299B1 (en) | 2020-02-11 |
| JP2017020446A (en) | 2017-01-26 |
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