JPH02126089A - Freezing and drying apparatus - Google Patents

Abstract

PURPOSE:To heat a whole matter to be dried to a temperature as high as possible of limiting temperature or lower in both the outer surface and the center by disposing heating plates on and underneath tray group in which many trays each containing the matter to be dried are brought into close contact with each other, and disposing cooling means on the four peripheral surfaces. CONSTITUTION:A heating system including a heater 15, a heat medium pump 16 and a heat medium pipe 17 and a cooling system including a cooler 18, a refrigerant pump 19 and a refrigerant pipe 20 are operated during freezing and drying works to heat heating plates 12, 13 and to cool cooling plates 14a, 14b, 14c, 14d. The heating system is so controlled that the center of matter to be dried in a tray 11 is heated to a temperature as high as possible of a limiting temperature or less at the center of the matter to be dried in the tray 11 by the plates 12, 13. Since the outer surface of the matter to be dried is apprehended to become high temperature by this heating, the cooling system reduces the incoming heat quantity of the outer surface to be controlled to suppress the temperature to the temperature as high as possible of the limiting temperature or lower similarly to that of the center.

Description

[Detailed description of the invention] (Industrial application field) This issue 8A relates to a freeze drying device.

(Prior Art) In a freeze-drying apparatus, a tray containing all the materials to be dried, such as various solutions (more specifically, an open container such as an ampoule or a vial containing the material to be dried, is heated while maintaining the material in a frozen state). The atmosphere in the sealed tank is reduced in pressure, whereby moisture contained in the material to be dried is sublimated, and the material to be dried is dried in a frozen state.

In such freeze-drying, when moisture and the like sublimate from the material to be dried, heat of sublimation is removed from the material to be dried, thereby further cooling the material to be dried. When the material to be dried is cooled, the external power efficiency decreases accordingly.

In order to prevent this decrease in sublimation efficiency, K is the temperature at which the material to be dried during freeze-drying is kept at a critical temperature & (i.e., the upper limit of the temperature at which there is no risk of quality deterioration due to defoaming and foaming of the water sea or deterioration of the melted material, etc.). ) and below, it is desirable to maintain the temperature as high as possible. Therefore, conventional measures have been taken to heat the material to be dried in the tray by placing heating plates above and below the tray and using the heating plates to heat the material to be dried in the tray during freeze-drying. At this time, if the tray is supported by a lower heating plate, the material to be dried is heated by contact heat conduction from the lower heating plate and heat radiation from the upper heating plate, and the tray is heated by a suitable support member. When the object to be dried is placed floating between the upper and lower support plates, the object to be dried is heated by O heat radiation from both the upper and lower heating plates.

(Problems to be Solved by the Invention) According to the conventional measures as described above, the temperature of the material to be dried can be increased by heating with a heating plate, and the temperature can be kept as high as possible below the limit temperature. It appears that the sublimation efficiency, ie the drying rate, can be significantly increased.

However, in reality, the outer periphery of the object to be dried near the outer edge of the tray receives more heat than the center of the object due to heat transfer from the inner wall of the sealed tank and the outer edge of the tray. It gets hot. Therefore, of course Km
Since the temperature Ill' at the outer periphery of the dried material must be maintained below the critical temperature, the central part can only be heated to a slightly lower temperature, and the sublimation efficiency, that is, the drying rate, in this central part is very low. Can't rise.

The present invention provides a freeze drying apparatus that eliminates all of the drawbacks of the conventional methods described above and is capable of heating the entire object to be dried, that is, both the outer periphery and the center, to a temperature as high as possible below the limit temperature. Its purpose is to.

(Means for Solving the Problems) In order to achieve the above-mentioned object, according to the present invention, a tray containing a material to be dried or a group of such trays that are mutually shuttled is heated vertically. A freeze-drying device is provided in which plates are arranged and cooling means are arranged around the four circumferences.

(Function) According to the configuration according to the present invention (the tray group will be described later), during freeze-drying, the upper and lower heating plates heat the central part of the material to be dried in the tray to a temperature as high as possible below the limit temperature. At the same time, the material to be dried is heated to such an extent that the temperature is raised, and at the same time, cooling means is applied to the outer periphery of the material to be dried, where there are many heat input pipes than the center and the temperature may become high due to this heating. By operating the outer periphery, the amount of people passing through the outer periphery is reduced and the temperature is kept as high as possible, below the same limit temperature as the center. The temperature laK can be maintained as high as possible below the temperature laK, and therefore the sublimation efficiency of the entire material to be dried, that is, the drying rate, can be maintained at a high value.

Regarding a group of trays in which many of the trays are attached to each other,
In terms of heat balance, this 1 can be considered as one large tray, so that the same effect as in the case of a single tray as described above is achieved.

(Example) Hereinafter, an example of the present invention will be described with reference to the drawings.

FIG. 1 represents an embodiment of a freeze-drying apparatus according to the invention. This freeze-drying equipment consists of a sealed tank io indicated by a broken line.
has. This closed tank lO has a tray l'j inside it.
It has a door (not shown) for loading and unloading, and is connected to an exhaust system (also not shown) for bringing the atmosphere inside into a reduced pressure state, and is further involved in freeze-drying work as necessary. Includes other members. Inside the closed tank lθ,
Horizontal upper heating plate/U and lower heating plate 13 parallel to each other
When the tray// is placed in the closed tank 10, it is placed on the lower heating plate 13 as shown in FIG. 7, or on a suitable support as shown in FIG. Depending on the material /ja, between the upper heating plate 12 and the lower heating plate /JCI,
arranged horizontally.

The V-closed cypress lO further includes a cooling plate no lIa, /! as a cooling means. b, /4tc, /! d (the clear 9th, lg C, and l dami are completely omitted from the illustration) are distributed. Cooling plate/
Da a, / da b, l tei c, / da d each extend vertically around the four circumferences of the tray 1 accommodated in the closed tank 10.

In detail, cooling plates a and l≠b are located on the left and right sides of the tray horn, respectively, and cooling plates 111C and /ud (not shown) are located on the front and rear of the tray, respectively.

The upper and lower heating plates 13 each have an internal passageway (not shown) connected to a heating medium piping equipped with a heater 15 and a heating medium pump 16 located outside the W, flash grating 10. It has a heating medium pipe/7f and circulates through the heating medium, which generates heat. Similar to this, cooling plate /4(a, /!b,
/! c, /4td is a refrigerant pipe equipped with a cooling ffi/ and a refrigerant pump 19 located outside the closed tank 10;
It has an internal passage (not shown) connected to 〇, and can be cooled by the refrigerant circulating through the entire refrigerant pipe 20. Although not shown, the cooler/S and refrigerant pump l? An appropriate refrigerator can be used for Q.

The material to be freeze-dried (not shown) is stored in an open container U/ such as an ampoule or a vial placed on a tray //, or directly into the tray // (not shown). be accommodated.

In the above-described freeze-drying apparatus, the freeze-drying operation is performed in exactly the same manner as in the conventional apparatus, except for the method of maintaining the temperature of the material to be dried. Therefore, to explain the unique temperature maintenance method, during the freeze-drying operation, the heater 15. The heating system including the heat medium pump 16 and the heat medium piping 17 and the cooling system including the cooler 1g1 refrigerant pump 19 and the refrigerant pipes 20 are fully operational, heating plates is and i3 are heated, and the cooling plate/4a is heated. , /4<b, /'4'c, /4d are cooled. At this time, the heating system uses upper and lower heating plates/2°13 to ensure that the central part of the material to be dried in tray ii (the material to be dried at a location t away from the outer edge of tray ll) is below the limit temperature. The temperature is controlled to be as high as possible. Depending on this heating, the outer periphery of the object to be dried (the object near the outer edge of the tray) may receive more heat than the center and become hotter, so the cooling system
Control is performed so as to reduce the amount of heat input to the outer circumference and keep the temperature as high as possible below the same limit temperature as that of the center.

FIG. 3 illustrates a semi-continuous freeze dryer M as another embodiment of the freeze dryer according to the invention.

This device includes an inlet gate valve 2, a preparation chamber 3, a preparation chamber gate valve 211. , freeze-drying operation S1, a take-out chamber gate valve roller, a take-out chamber body, and an outlet gate valve 2S are connected in series in this order. Inlet gate valve 28 Outside, inside the preparation chamber 3, inside the freeze-drying chamber 5, inside the take-out chamber core, and outside the outlet gate valve 28, there are conveyor members 29°3o, such as roller conveyors. yi, ys and 33 are installed, respectively. When the inlet gate valve 5yfkJ and the conveying member 30 are operated, the tray // is carried into the preparation chamber J from the inlet side, and then the inlet gate valve 3 is closed and the preparation chamber gate valve 44i is moved. Upon opening and actuation of the transport member 30.3/, the tray 71 is transferred from inside the compartment 3 into the freeze-drying operation 5.

Thereafter, the loading chamber gate valve moss is closed, and the tray// is thus opened from the outside of the freeze-drying apparatus to the freeze-drying chamber S without substantially impairing the atmosphere inside the freeze-drying chamber S. It can be carried inside. Similarly, transport members 3, 3, 3
By proper operation of 3 and proper closure of gate valve roller 2S, the freeze-drying chamber 5 can be closed without substantially impairing the atmosphere inside the tray/lF'i and the freeze-drying chamber 5. It can be transported from inside the freeze-drying chamber to the outside of the freeze-drying chamber.

When performing freeze-drying work 1 in the freeze-drying chamber 5, the tray // is supported at a constant F by the conveying member 31, or is placed on the conveying member 3 and moved from the preparation chamber side to the outside of the unloading chamber by its operation. It moves slowly. Inside the freeze dryer 25, there are the aforementioned heating plate saws colored above and below the conveying member 3/.

/3 and the same upper heating plate saw A and lower heating plate /JA are distributed, and the cooling plates /Qa, /! b,
/+c, /Qd and the same rear end cooling plate/! Aa
, a front end cooling plate/4'Ab, a first side cooling plate Lda Ac and a second side cooling plate/IA (L are arranged. However,
In order to simplify the drawing, the illustration of the second side cooling plate/4 (All is omitted).

These cooling plates /HiroAa, /4Ab, /! Ac.

/1IA (l is arranged so as to surround the four circumferences of the tray /l that is fixed and moved across during the freeze-drying operation.

In the embodiment shown in FIG. 3, unlike the embodiment shown in FIG. When configured and retracted, the transport member, 30.3! ,,3
It is located in a place where it will not interfere with the transport of the tray/l by the machine.

In the embodiments shown in FIGS. 7 and 2, seven trays on which many open-hole containers are placed are used. It is also possible to use trays that are housed in each other, and a group of trays in which many of these trays are brought into close contact with each other can also be used as seven large trays.

(Effects of the Invention) The freeze-drying apparatus according to the present invention can heat the entire object to be dried housed in the tray to a temperature as high as possible below the limit temperature during the freeze-drying operation, and therefore the sublimation movement of the object to be dried can be heated to a temperature as high as possible below the limit temperature. That is, it has the effect of improving the drying rate.

[Brief explanation of the drawing]

FIG. 7 shows a first embodiment of the freeze-drying apparatus according to the invention. FIG. 2 represents a modification of the embodiment of FIG. FIG. 3 shows a first embodiment of the freeze-drying apparatus according to the present invention. In the drawing, 10 is a tray, i2. icoA. /, 3. /3A is a heating plate, /4<a, /4tb, /4C
Mua, /daAb, /damC indicate cooling means. Figure 1 Figure 2

Claims (1)

[Claims] Heating plates are arranged above and below a tray containing objects to be dried or a group of trays in which many such trays are brought into close contact with each other,
A freeze-drying device with cooling means arranged around all four sides.