JP6771334B2 - Freeze-dryer seal structure - Google Patents

Description

The present invention relates to a seal structure of a joint portion in a freeze-dryer for manufacturing pharmaceuticals, foods, chemical products, etc. by freeze-drying a liquid-adjusted material to be dried.

Freeze-dryers, especially those applied to the manufacture of pharmaceuticals and foods, are strongly required to prevent contamination hazards and ensure sterility.

Conventionally, in order to meet such a requirement, an O-ring and an inflatable gasket are double-sealed between the chamber and the door constituting the freeze-dryer, and the O-ring and the inflatable gasket are provided with the door closed. A barrier system for a freeze-dryer that fills an inert gas such as nitrogen gas in an annular space formed between the two is proposed (see, for example, Patent Document 1).

In Patent Document 1, as an effect of the barrier system, even when the sanitary treatment of the isolator in which the freeze-dryer is arranged and the freeze-drying operation of the material to be dried are performed at the same time, the chemistry for sanitary treatment in the chamber is performed. It is stated that the attraction of substances can be prevented.

Special Table 2010-509563

However, in the barrier system described in Patent Document 1, an inert gas is filled in an annular space formed between the O-ring and the expandable gasket, and the pressure of the inert gas is used for sanitary treatment into the chamber. Since it prevents the attraction of chemical substances, its effect is exhibited only when the soundness of the O-ring and the expandable gasket is ensured. That is, when one or both of the O-ring and the expandable gasket deteriorate and their sealing function deteriorates, the pressure of the inert gas filled in the annular space causes the inert gas and the chemical substance for sanitary treatment to be released. It is easily drawn into the chamber, resulting in contamination of the chamber with bacteria and sanitary chemicals in the inert gas.

In addition, sterilization of the inert gas filled in the annular space and the inert gas for expanding the expandable gasket requires large-scale and expensive sterilization equipment, so it is practically adopted. Can not do it.

The present invention has been made to solve such a problem of the prior art, and an object of the present invention is to provide a seal structure for a freeze-dryer capable of preventing contamination hazards and ensuring sterility with a simple configuration. There is.

In the present invention, in order to solve the above problems, the freeze-drying chamber is composed of a combination of a plurality of parts joined via a flange, and the plurality of parts are concentrically arranged on the joint surface of the flange. in one O-ring and the seal structure of the freeze-dryer is fastened by bolts through the flange, at a position not and set portion and communicating said two O-rings between the two O-ring in the joint surface of the flange and formed a ring-shaped groove such that said pressure ring groove is lower than the pressure in the freeze-drying chamber, characterized in that it comprises a vacuum pump for evacuating the air in the ring-shaped groove ..

According to this configuration, two O-rings are concentrically arranged on the joint surface of the flange, and the air in the ring-shaped groove formed between these two O-rings is evacuated by a vacuum pump. The joint surface of a plurality of parts constituting the above can be kept at a negative pressure at all times, and foreign matter can be prevented from entering the freeze-drying chamber from the joint surface. If the inside of the inner O-ring setting part is evacuated, it becomes difficult to control the degree of vacuum inside the freeze-dryer, and if the outside of the outer O-ring setting part is evacuated, the inner O-ring is evacuated. When the ring deteriorates, it is not possible to prevent the inflow of outside air from the middle portion of the two O-rings into the vacuum dryer. Therefore, if the soundness of the two O-rings is maintained by evacuating the air in the ring-shaped groove formed between the two O-rings, of course, if the two O-rings are evacuated, Even if one or both of them are deteriorated, it is possible to prevent contamination hazards and ensure sterility in the freeze-drying chamber without adversely affecting the control of the degree of vacuum in the freeze-drying chamber.

According to the present invention, the degree of vacuum in the ring-shaped groove is kept equal to or lower than the degree of vacuum in the freeze-drying chamber, so that foreign matter can be completely prevented from entering the freeze-drying chamber from the joint surface of the flange. ..

Further, in the present invention, in the seal structure of the freeze-dryer having the above configuration, the vacuum pump that evacuates the air in the ring-shaped groove is provided separately from the vacuum pump that evacuates the air in the freeze-drying chamber. It is characterized by.

According to the present invention, since a vacuum pump that evacuates the air in the ring-shaped groove and a vacuum pump that evacuates the air in the freeze-drying chamber are separately provided, control for adjusting the degree of vacuum in the ring-shaped groove is provided. Is no longer required, and the control system of the vacuum pump can be simplified.

Further, in the present invention, in the seal structure of the freeze-dryer having the above configuration, an O-ring having a large wire diameter is arranged on the inner peripheral side of the flange, and an O-ring having a small wire diameter is arranged on the outer peripheral side of the flange. It is characterized by that.

According to the present invention, since the O-ring having a large wire diameter having a high sealing effect on the joint surface is arranged on the inner peripheral side of the flange, the joint surface of the flange can be provided with high sealing property. In addition, since an O-ring with a small wire diameter is placed on the outer peripheral side of the flange, it is possible to form a ring-shaped groove on the joint surface of the flange without increasing the size of the flange, and the flange and thus the freeze-drying cabinet can be downsized. Can be planned.

Further, the present invention is characterized in that, in the seal structure of the freeze-dryer having the above structure, the freeze-dryer has an upright cylindrical tube structure.

A freeze-dryer having an upright cylindrical tube structure has a larger number of parts joined via a flange than a box-shaped freeze-dryer. Therefore, if a sealing failure occurs at the joint of each part, a contamination hazard occurs. It tends to be difficult to ensure sterility. When the present invention is applied to a freeze-drying cabinet having an upright cylindrical tube structure, even if a sealing failure occurs at the joint of each part, contamination hazards are prevented and sterility is ensured. The practicality of the freeze-drying cabinet having a tube structure can be further enhanced.

According to the present invention, two O-rings are concentrically arranged on the joint surface of the flange, and the air in the ring-shaped groove formed between the two O-rings is evacuated by a vacuum pump. It is possible to prevent contamination hazards and ensure sterility for a freeze-dryer composed of a plurality of parts joined via a plurality of parts.

It is a block diagram of the freeze-dryer which concerns on embodiment. It is sectional drawing of the main part which shows the seal structure of the freeze-dryer which concerns on a conventional example. It is sectional drawing of the main part which shows the seal structure of the freeze-dryer which concerns on embodiment.

Hereinafter, embodiments of the seal structure of the freeze-dryer according to the present invention will be described with reference to FIGS. 1 and 2.

First, in the freeze-dryer according to the embodiment, as shown in FIG. 1, a freeze-drying chamber for freeze-drying a liquid material to be dried is formed by an upright cylindrical tube 1, and the tube 1 is formed. A tubular jacket 2 for circulating the heat medium is provided on the outer periphery. The inside of the jacket 2 is provided with a plurality of stages (three stages in the example of FIG. 5) of heat medium flow paths 2a, 2b, and 2c divided in the length direction of the tube 1. The heat medium flow paths 2a, 2b, and 2c of each of these stages are provided with an inlet pipe 20 and an outlet pipe 21, respectively, and each of these inlet pipes 20 and outlet pipes 21 is provided with a refrigerator d and a heat exchanger. The conduit f of the temperature control device including e and the heater h is connected, and a heat medium adjusted to a predetermined temperature is supplied to each of the heat medium flow paths 2a, 2b, and 2c of each stage.

A dome-shaped duct 3 is provided in the upper part of the tube 1, and the duct 3 is connected to a vacuum exhaust system (not shown) equipped with a vacuum pump and a cold trap via a valve 30. In the duct 3, a pipe 5 extending from the material tank t2 attached to the machine frame F is arranged, and at the tip thereof, a dispensing nozzle 70 that injects a liquid material to be dried onto the inner wall surface of the tube 1. Is installed.

A conduit 90 extending from the distilled water tank t3 attached to the machine frame F is connected to the pipe 5, and a switching valve V4 is provided at the confluence of the pipe 5 and the conduit 90. Therefore, by switching the switching valve V4, the material to be dried or distilled water can be appropriately sprayed from the dispensing nozzle 70 onto the inner wall surface of the tube 1. Reference numeral p2 in the figure indicates a water supply pump that supplies distilled water stored in the distilled water tank t3 to the dispensing nozzle 70 through the conduit 90, the switching valve V4, and the pipe 5.

The upper end of the tube 1 and the lower end of the duct 3 are joined via flanges 51a and 51b, and are fastened with bolts (not shown). Further, the upper end of the duct 3 and the lower end of the pipe provided with the valve 30 are joined via flanges 52a and 52b, and are fastened with bolts (not shown). Further, the duct 3 of this example is composed of a lower member 3a and an upper member 3b, and the upper end of the lower member 3a and the lower end of the upper member 3b are joined via flanges 53a and 53b, and bolts (not shown). It will be concluded at.

On the other hand, the lower part of the tube 1 is connected to the collection chamber 4 of the dry bulk formed in a funnel shape via the connecting pipe 43. The collection chamber 4 is connected to an inlet 82 of a crushing device 8 for finely crushing dry bulk via a transport cylinder 41, and crushing crushed by the crushing device 8 is on the outlet 83 side of the crushing device 8. A cyclone separation device 81 that separates an object into air and powder is connected. The reduced diameter portion of the recovery chamber 4 is provided with a jet nozzle 42 that roughly pulverizes the cylindrical dry bulk collected from the tube 1 by air pressure.

The jet nozzle 42 generates a swirling flow centered on the axis of the recovery chamber 4 in the recovery chamber 4, and the swirling flow creates a cylindrical dry bulk that falls from the tube 1 into the recovery chamber 4. Coarsely grind. Further, valves V1 and V2 are provided in the small diameter portion of the recovery chamber 4 to sequentially discharge the dry bulk roughly crushed by the jet nozzle 42 to the crushing device 8 side via the transport cylinder 41.

Further, a take-out pipe 6 provided with the valve V3 is connected between the valve V1 and the valve V2, and the other end of the take-out pipe 6 is connected to a recovery tank t1 for collecting the unfrozen material to be dried. ing. The unfrozen material to be dried stored in the recovery tank t1 is pumped up by the pumping pump p1 and returned to the material tank t2 through the pipeline 6a.

The lower end of the tube 1 and the upper end of the connecting pipe 43 are joined via flanges 54a and 54b, and are fastened with bolts (not shown). Further, the lower end of the connecting pipe 43 and the upper end of the recovery chamber 4 are joined via flanges 55a and 55b, and are fastened with bolts (not shown).

Hereinafter, the seal of the freeze dryer is applied between the flanges 51a and 51b, between the flanges 52a and 52b, between the flanges 53a and 53b, between the flanges 54a and 54b, and between the flanges 55a and 55b. The structure will be described in comparison with the prior art. In the following, the seal structure of the freeze-dryer provided between the flanges 51a and 51b will be described as an example, but the same applies to the seal structure of the freeze-dryer provided between the other flanges.

FIG. 2 shows a conventional seal structure in a freeze-dryer in which a freeze-dryer is formed by holding an upright cylindrical tube 1. As shown in FIG. 2, conventionally, one O-ring 60 having an inner diameter slightly larger than the inner diameters of the flanges 51a and 51b is arranged between the joint surfaces of the flanges 51a and the joint surfaces of the flanges 51b. The flange 51a and the outer peripheral portion of the flange 51b are fastened with bolts 56.

Even with such a seal structure, if the soundness of the O-ring 60 is maintained, no special problem occurs. However, when the O-ring 60 deteriorates and its sealing function deteriorates, the tube is adjusted to a predetermined degree of vacuum, for example, about 1 Pa to 100 Pa, through a gap between the joint surface of the flange 51a and the joint surface of the flange 51b. Outside air is drawn into 1 and it becomes impossible to guarantee the prevention of contamination hazards and the assurance of sterility.

On the other hand, in the seal structure of the freeze-dryer according to the embodiment, as shown in FIG. 3, the inner diameters of the flanges 51a and 51b are between the joint surface of the flange 51a and the joint surface of the flange 51b to be joined to each other. The first O-ring 61 having a slightly larger inner diameter and the second O-ring 62 having an inner diameter larger than that of the first O-ring 61 are concentrically arranged, and the outer peripheral portions of the flange 51a and the flange 51b are arranged concentrically. , Bolt 56 is used for fastening.

As the first O-ring 61, one having a wire diameter larger than that of the second O-ring 62 is used. As described above, in the seal structure of the freeze-dryer according to the embodiment, since the O-ring having a large wire diameter is arranged on the inner peripheral side of the flanges 51a and 51b, the joint surface of the flanges 51a and 51b is provided with high sealing property. be able to. Further, since the second O-ring 62 having a wire diameter smaller than that of the first O-ring 61 is arranged on the outer peripheral side of the first O-ring 61, the flanges 51a and 51b are not enlarged and the flanges 51a and 51b are not enlarged. It is possible to form a ring-shaped groove on the joint surface of the freeze-drying chamber, and the freeze-drying chamber can be miniaturized.

In the example of FIG. 3, a first O-ring 61 having a wire diameter larger than that of the second O-ring 62 was used, but conversely, the second O-ring 62 was the first. A wire diameter larger than that of the O-ring 61 can also be used. Further, as the first O-ring 61 and the second O-ring 62, those having the same wire diameter can be used.

Further, in the seal structure of the freeze dryer according to the embodiment, as shown in FIG. 3, the first and second O-rings 61 and 62 are set between the first and second O-rings 61 and 62. A ring-shaped groove 63 that does not penetrate the portion is formed. An exhaust hole 64 communicating with the ring-shaped groove 63 is formed in the flange 51b, and the other end of the exhaust pipe 65, one end of which is connected to the vacuum pump P, is connected to the exhaust hole 64. Therefore, the air in the ring-shaped groove 63 is evacuated by the vacuum pump P.

Since the seal structure of the freeze-dryer according to the embodiment is configured in this way, the joint surfaces of the flanges 51a and 51b can be kept at a negative pressure at all times, and the joint surfaces of the flanges 51a and 51b can be passed through the joint surfaces. Foreign matter that is about to enter the tube 1 can be discharged to the outside of the system. Therefore, it is possible to prevent contamination hazards in the tube 1 not only when the soundness of the two O-rings 61 and 62 is maintained, but also when one or both of the two O-rings 61 and 62 deteriorate. And ensuring sterility can be guaranteed.

That is, if the inside of the setting portion of the inner O-ring 61 is evacuated, it becomes difficult to control the degree of vacuum in the tube 1, and if the outside of the setting portion of the outer O-ring 62 is evacuated, the inside is evacuated. When the O-ring 61 deteriorates, it is not possible to prevent the inflow of outside air from the intermediate portion of these two O-rings 61 and 62 into the vacuum dryer. On the other hand, if the air in the ring-shaped groove 63 formed between the two O-rings 61 and 62 is evacuated, such an inconvenience cannot occur. Therefore, the soundness of the two O-rings 61 and 62 If one or both of the two O-rings 61 and 62 deteriorates, of course, the tube 1 is contaminated without adversely affecting the control of the degree of vacuum in the tube 1. It is possible to prevent hazards and ensure sterility.

Since the freeze-dryer composed of the upright cylindrical tube 1 has a larger number of parts joined via the flange than the box-shaped freeze-dryer, the seal structure of the freeze-dryer according to the embodiment is applied. By doing so, the prevention of contamination hazards and the assurance of sterility can be ensured, and its practicality can be enhanced.

As the vacuum pump P, a vacuum pump P having the ability to reduce the pressure inside the ring-shaped groove 63 to the same as or slightly lower than that inside the tube 1 is selected. In order to prevent foreign matter from entering the tube 1, it is preferable that the difference between the degree of vacuum in the ring-shaped groove 63 and the degree of vacuum in the tube 1 is large, but for that purpose, a large and expensive vacuum pump is used. You will need it. In the present embodiment, these interests are weighed and the vacuum pump P having the ability to reduce the pressure inside the ring-shaped groove 63 to the same as or slightly lower than that inside the tube 1 is selected. For example, when the degree of vacuum in the tube 1 at the time of freeze-drying of the material to be dried is 5 Pa, a vacuum pump P capable of evacuating the degree of vacuum in the ring-shaped groove 63 to about 1 Pa is selected. The vacuum pump P may be configured to control on / off and drive conditions by a control device (not shown), or may be configured to manually turn on / off without being controlled by the control device.

In the seal structure of the freeze-dryer according to the embodiment, the inside of the ring-shaped groove 63 is evacuated to the same or lower pressure than the inside of the tube 1, so that foreign matter enters the freeze-drying chamber from the joint surface of each flange. Can be completely prevented.

The vacuum pump P can be provided separately from the vacuum pump that evacuates the air in the tube 1. In this way, the control system for adjusting the degree of vacuum in the ring-shaped groove 63 becomes unnecessary, so that the control system of the vacuum pump P can be simplified.

For the operation of the freeze-dryer according to the embodiment, refer to the description of Japanese Patent No. 549586865.

The present invention relates to a seal structure of a freeze-dryer applied to a flange, and the configuration of other parts can be appropriately changed regardless of the above embodiment.

The present invention can be used in a freeze-dryer used for freeze-drying pharmaceuticals, foods, chemical products and the like.

1 Tube 2 Jacket 2a, 2b, 2c Heat medium flow path 3 Duct 4 Recovery chamber 5 Piping 6 Extraction pipe 8 Crusher 20 Inlet pipe 21 Outlet pipe 30 Valve 41 Conveyor cylinder 42 Jet nozzle 51a, 51b Flange 52a, 52b Flange 53a, 53b Flange 54a, 54b Flange 54a, 54b Flange 56 Bolt 60, 61, 62 O-ring 65 Exhaust pipe 70 Dispensing nozzle 81 Cyclone separator d Refrigerator e Heat exchanger h Heater f Pipe line t1 Recovery tank t2 Material tank t3 Distilled water tank

Claims (4)

The lyophilizer consists of a combination of a plurality of parts joined via a flange, and the plurality of parts are concentrically arranged on the joint surface of the flange by two O-rings and bolts via the flange. In the seal structure of the lyophilizer to be fastened
A ring-shaped groove formed between the two O-rings on the joint surface of the flange and at a position not communicating with the setting portion of the two O-rings .
As the pressure of the ring-shaped groove is lower than the pressure in the freeze-drying chamber, the seal structure of the freeze-dryer, characterized in that it comprises a vacuum pump for evacuating the air in the ring-shaped groove. Vacuum pump for evacuating the air in the ring-shaped groove, the sealing structure of the freeze-drying apparatus according to claim 1, characterized in that it comprises an air in said freeze drying cabinet separate from the vacuum pump to evacuate .. The freeze-dryer according to claim 1 or 2 , wherein an O-ring having a large wire diameter is arranged on the inner peripheral side of the flange, and an O-ring having a small wire diameter is arranged on the outer peripheral side of the flange. Seal structure. The seal structure of the freeze-dryer according to any one of claims 1 to 3 , wherein the freeze-drying cabinet has an upright cylindrical tube structure.