KR100889789B1 - Machine for Frozen Drying - Google Patents

Abstract

The present invention provides a freeze dryer for freeze-drying a liquid frozen dried product, comprising: a chamber having an inner space; A vessel disposed in the chamber and open at the top; A liquid nitrogen inlet provided in the chamber to supply liquid nitrogen to the container; A nitrogen gas outlet provided in the chamber for discharging nitrogen gas formed by vaporizing liquid nitrogen in the container to the outside of the chamber; A passive dry spray nozzle installed in said chamber to inject said liquid frozen structure into a container containing said liquid nitrogen; Heating means for heating the vessel to dry the frozen dried matter in the vessel; And, it provides a lyophilizer comprising a vacuum pump for making the space inside the chamber into a vacuum.

Dryer, Chamber, Liquid Nitrogen, Nitrogen Gas, Vacuum Pump

Description

Freeze Drying {Machine for Frozen Drying}

1 is an interior view of a lyophilizer according to an embodiment of the present invention.

Figure 2 is an internal view of the container removed from the lyophilizer shown in FIG.

3 is a block diagram illustrating a system of a lyophilizer according to an embodiment of the present invention.

 4 is a detailed view of the container shown in FIG. 1.

Explanation of symbols on the main parts of the drawings

10 chamber 11 both side walls

12: upper wall 20: container

21: catching part 30: liquid nitrogen inlet

31: liquid nitrogen storage tank 40: nitrogen gas outlet

41: nitrogen gas storage tank 42: valve

50: spray nozzle for the frozen building 51: storage tank for the frozen building

60: heating means 61: shelf

62: heat fluid supply unit 63: hydraulic cylinder

64: piping 70: vacuum pump

75 condenser 81 roller

82: motor

The present invention relates to a lyophilizer, and more particularly, to a lyophilizer having an improved structure so that preliminary synergism and lyophilization can be performed in one chamber.

Freeze-drying is a type of drying, as is well known, that freezes frozen matter, ices the water inside it, and then sublimates the ice inside the frozen matter while lowering the partial pressure of water vapor in the atmosphere. It means to dry the frozen building by discharging it into steam. When energy is supplied to the ice under low pressure, it is not sublimed but instead sublimed directly into water vapor. This method is a drying method that dries moisture inside the frozen dried material using this principle. Sublimed ice crystals leave voids inside the passive building, so the dried material contains a myriad of pores, which can be easily absorbed by water in the future and left to dry before rehydration. It is easily restored.

This lyophilization method has the disadvantage that the equipment is expensive, but is widely used for drying products that require heat-sensitive products, products in the form of particulates, and products requiring rapid and complete rehydration.

One field in which such lyophilization is applied is in the field of drying medicines. Injecting medicines into the human body includes injection by injection, injection by breath, injection by dose, and the like. Among them, injection is a method of injecting a chemical solution directly into a human blood vessel by injection, and inhalation is a method of injecting a dry powder of medicine by breathing. It is injected into the human body through capillaries. And injection by taking is a way that the drug is taken through the mouth and esophagus and then absorbed by the digestive system.

Among these methods, injection is the most effective, but the injection is cumbersome, such as the need to have someone to perform the injection, but in the case of the method of inhalation by inhalation can easily inject the medicine into the patient's body In addition, there is an excellent advantage in terms of absorption of the chemical solution as well as injection by injection, and in recent years, interest in the chemical powder that can be injected by respiration has increased. In particular, it is very difficult to use injections in extreme situations such as wartime, and thus, the demand for taking medicine in the form of a chemical powder that can be injected by respiration is very high in the case of military use.

Powder medicines that can be injected by respiration are mainly manufactured by spray drying and spray freeze drying. Among these spray drying and spray freeze drying methods, the spray freeze drying method is known as an advantageous method for the preparation of powder having a particle size of 5-10 μm suitable for respiration.

Spray freeze drying refers to a method of spraying a liquid frozen dry product into particles of a predetermined size by a sprayer in a low temperature chamber to freeze the injected frozen dry material and then freeze-drying the frozen frozen dry product again. Conventional spray freeze drying consists of two stages of preliminary freezing and freeze-drying to spray and freeze the liquid lyophilisate, and the preliminary freezing and freeze drying are performed by different equipment.

Therefore, a device for preliminary freezing and a separate equipment for lyophilization are required, which is directly connected to a cost problem and causes a problem of increasing the manufacturing cost of the freeze-dried product. In addition, there is a problem that the space for accommodating the equipment increases as separate equipment is used for each step. On the other hand, when preliminary freezing and freeze drying are performed on separate equipment, it is necessary to transfer the pre-frozen frozen freeze to the freeze-drying machine. There was also a problem that hassle, such as having to finish the transport operation.

The present invention has been made to solve the problems of the conventional spray freeze drying method described above, and an object thereof is to provide a freeze dryer that can be freeze-dried preliminary freezing in one chamber.

In order to achieve the above object, the present invention,

In the freeze dryer for freeze-drying the liquid frozen dried matter,

A chamber having a space formed therein, a container having an upper surface opened therein, a liquid nitrogen inlet formed at an upper wall of the chamber so as to introduce liquid nitrogen into the container, and a liquid in the container. A nitrogen gas outlet formed at one side of an upper wall of the chamber to discharge nitrogen gas generated by nitrogen vaporization to the outside of the chamber, and an upper wall of the chamber to inject the liquid passive dry matter into a container containing the liquid nitrogen. And a vacuum pump formed to vacuum the space inside the chamber, the heating means being formed on the lower surface of the inside of the chamber so as to heat the container for drying the dried object in the container. It is configured to include, the container is hooked to be installed in the chamber on the outer peripheral surface of the open upper surface Sex and, inside of the chamber is formed in the shape of a rectangular parallelepiped, a plurality of rollers are formed at regular intervals to both side walls of the chamber, the engaging portion of the container can be secured, it is possible to rotate. The roller is provided with a motor capable of forward and reverse rotation to apply vibration to the container, and the heating means is provided with a pipe for circulating the heat fluid inside the shelf, the pipe is installed in the inside of the shelf circulates the heat fluid The heat fluid supply unit is installed on the outside of the chamber, the heating means is adjustable in height to allow access and separation from the container, the hydraulic cylinder is mounted on the lower surface of the shelf for adjusting the height of the heating means It is characterized in that the height can be adjusted by the cylinder.

Hereinafter, an embodiment of the present invention will be described in detail with reference to the accompanying drawings.

1 is an internal view of a freeze dryer according to an embodiment of the present invention, Figure 2 is an internal view of a state in which the container is removed from the freeze dryer shown in Figure 1, Figure 3 is a freezing according to an embodiment of the present invention A block diagram for explaining the system of the dryer, and FIG. 4 is a detailed view of the container shown in FIG.

The freeze dryer according to an embodiment of the present invention, as shown in Figures 1 to 3, the chamber 10, the vessel 20, the vessel vibrating means, the liquid nitrogen inlet 30, nitrogen gas outlet 40 and And a passive building spray nozzle (50), a heating means (60) and a vacuum pump (70).

The chamber 10 corresponds to the main body of the lyophilizer of the present embodiment, and an internal space having a rectangular parallelepiped shape is provided therein.

Rollers 81 are provided on both side walls 11 of the chamber 10. The plurality of rollers 81 are provided on both side walls 11 of the chamber 10 along the front and rear directions of the chamber 10. The rollers 81 are arranged to be rotatable with respect to both side walls 11 of the chamber 10.

The front of the chamber 10 is provided with a door (not shown).

The vessel 20 is arranged in the chamber 10, the top of which is open. As illustrated in FIG. 4, upper and lower ends of the container 20 are provided with locking portions 21 extending in the outward direction of the container 20, so that the locking portions 21 are formed on the rollers 81. Are placed inside the chamber 10.

The container 20 may enter the inside of the chamber 10 through a door provided in the chamber 10, or may be carried out from the inside of the chamber 10 to the outside.

When the container 20 is placed in the chamber 10, the locking portion 21 of the container 20 may be placed on the roller 81 and then pushed in, and the container 20 may be pushed out of the chamber 10. You can do it the opposite way.

The vessel vibrating means includes motors 82 connected to the rollers 81 to shake the vessel. That is, motors 82 capable of forward and reverse rotation are connected to the rollers 81 to rotate the rollers 81. The rollers 81 rotate forward and backward by the motors 82 to allow the container ( 20) can be shaken.

As shown in FIGS. 1 and 2, the liquid nitrogen inlet 30 is provided at an upper portion of the vessel 20, and more specifically, is provided at an upper wall 12 inside the chamber 10. Liquid nitrogen is supplied into the vessel 20 through the liquid nitrogen inlet 30. As shown in the block diagram of FIG. 3, the liquid nitrogen inlet 30 is connected to a separate liquid nitrogen storage tank 31 so that the liquid nitrogen supplied from the liquid nitrogen storage tank 31 is the liquid nitrogen inlet. It is supplied to the container 20 through 30.

The nitrogen gas outlet 40 is for discharging the nitrogen gas formed by vaporizing the liquid nitrogen supplied to the vessel 20 through the liquid nitrogen inlet 30 to the outside of the chamber 10. As shown in the upper wall 12 of the chamber 10. In addition, as shown in FIG. 3, the nitrogen gas outlet 40 is connected to the nitrogen gas storage tank 41 so that the discharged nitrogen gas is stored. A valve 42 is provided in a pipe through which the discharged nitrogen gas moves to the nitrogen gas storage tank 41, and a separate pump (not shown) is provided to effectively discharge the nitrogen gas from the nitrogen gas outlet 40. It may be arranged.

The passive building injection nozzle 50 is installed on the upper wall 12 inside the chamber 10. The passive dry matter stored in the passive dry matter storage tank 51 is injected into the container 20 through the injection nozzle 50.

The passive dry material is sprayed through the passive dry spray nozzle 50.

The passive building injection nozzle 50 may be selected and used as appropriate injection nozzles on the market, the biggest consideration in the selection is the particle size of the passive building to be sprayed. The particle size of the passive building sprayed through the passive building injection nozzle (50) is determined according to the nature of the passive building, in the case of the drug solution is preferably 5-10 μm, the most effective particle size for injection by breathing Do.

Meanwhile, a separate injection nozzle end heating means may be provided for heating an end portion of the passive building injection nozzle 50 to which the passive dry material is injected, a process in which the passive dry material is sprayed from the passive building injection nozzle 50. This is because it may occur at the end of the frozen building injection nozzle 50 due to the low temperature in the chamber (10). In this case, the passive building casting injection nozzle 50 is blocked so that the heating means 60 is for heating the vessel 20. In order to dry the frozen building in the frozen state, it is necessary to apply heat to the frozen building.

The heating means 60 includes a shelf 61 and a heat fluid supply part 62.

The shelf 61 is installed to be accessible and spaced apart from the container 20. Access to and away from the container 20 of the shelf 61 may be by a variety of means, in this embodiment is made by the hydraulic device 63 as shown in Figures 1 and 2.

Inside the shelf 61, a pipe 64 for circulating a thermal fluid for applying heat to the vessel 20 is provided.

The heat fluid supply part 62 supplies the heat fluid to the pipe 64 provided in the shelf 61.

The vacuum pump 70 is a configuration for making the interior space of the chamber 10 into a vacuum state so that water inside the passive building can be sublimated directly from ice to water vapor in the process of drying the passive building.

On the other hand, the sublimated water vapor is also discharged together in the process of drying the passive building through the vacuum pump 70, it is preferable that a separate condenser (75, see Fig. 3) for condensing the discharged water vapor is also installed. Do.

Hereinafter, the function and operation of the freeze dryer according to the above-described embodiment will be described in detail.

In order to explain the function and operation of the lyophilizer of the present embodiment, it is easy to explain the operation step for lyophilizing the dried product. Hereinafter, the function of each component in each step according to the lyophilized step of the frozen product is described below. And to explain the action.

First, the container 20 is installed inside the chamber 10 through the door of the chamber 10. The container 20 is provided with a locking portion 21. The locking portion 21 is placed on the rollers 81 provided on both side walls 11 of the chamber 10, and then pushed in.

When the container 20 is installed inside the chamber 10, the door is closed to completely block the inside of the chamber 10 from the outside.

When the inside and the outside of the chamber 10 are closed from each other by closing the door, the liquid nitrogen is supplied to the container 20 through the liquid nitrogen inlet 30. At this time, the valve 42 provided in the pipe connected to the nitrogen gas outlet 40 is in a closed state to prevent nitrogen gas from being discharged through the nitrogen gas outlet 40.

The amount of liquid nitrogen supplied to the vessel 20 through the liquid nitrogen inlet 30 fills about 1 / 3-1 / 2 of the vessel 20, and the amount of liquid nitrogen is the temperature of the space inside the chamber 10. It can be adjusted to an amount that can be lowered enough to freeze at the same time that the passive building is sprayed.

When the liquid nitrogen is supplied to the vessel 20 and the temperature inside the chamber 10 becomes sufficiently low, the dried matter is sprayed through the passive building injection nozzle 50. The sprayed dry matter is to be accommodated in the container 20 in a frozen state immediately upon spraying.

At this time, by rotating the motor 82 connected to the rollers 81 forward and backward to shake the container (20). This is to prevent the frozen frozen frozen building from tangling with each other in the process of being accommodated in the container (20).

When the freeze-dried material is freeze-dried as much as the amount to be lyophilized, nitrogen gas is discharged to the outside of the chamber 10 through the nitrogen gas outlet 40. To do this, the valve 42 must be opened. When the valve 42 is opened, the vaporized nitrogen gas is discharged while the partial pressure of nitrogen gas in the chamber 10 falls, so that the liquid nitrogen is continuously vaporized, and the vaporized nitrogen gas is again chambered through the nitrogen gas outlet 40. Since the liquid is discharged to the outside of the 10, the liquid nitrogen does not remain in the container 20. However, some nitrogen gas remains inside the chamber 10.

When all of the liquid nitrogen in the vessel 20 is discharged, only the frozen passive dry matter remains inside the vessel 20. At this time, by operating the vacuum pump 70 to make the interior of the chamber 10 to a vacuum. At this time, all of the nitrogen gas remaining in the chamber 10 through the vacuum pump 70 may be discharged.

After making the interior of the chamber 10 vacuum by the vacuum pump 70, the shelf 61 is approached to the container 20 side to be in contact with the container 20 by using the hydraulic device 63. The vessel 20 is heated by circulating a heat fluid in the pipe 64 provided inside the shelf 61, and finally, heat is applied to the frozen structure in the frozen state.

When heat is applied to the frozen building, the ice in the frozen building melts, and under low temperature and low pressure, the ice does not melt, but sublimation occurs immediately. Is removed by sublimation with water vapor.

The sublimated water vapor inside the passive building is discharged to the outside of the chamber 10 by a vacuum pump and condensed through a condenser 75 separately provided.

As described above, in the process of removing the water inside the frozen building, the container 20 may be appropriately shaken to allow the water to be easily sublimed from the frozen building.

In this way, if all the moisture in the passive building is removed, the frozen structure in a dried state can be obtained.

In the above, the embodiment including the shelf and the heat fluid supply part 62 as the heating means has been described. However, the heating means is not limited thereto, and an appropriate means for heating the container 20 may be employed. The change of the heating means 60 is not outside the scope of the technical idea of the present invention.

In the above described the embodiment further includes a vibrating means of the vessel 20, even if there is no vibrating means to achieve the object of the present invention, the container 20, the freeze dryer without the vibrating means also It does not depart from the scope of the technical idea of the present invention.

Although the lyophilizer of the present invention has been described above based on the preferred embodiment, the technical idea of the present invention is not necessarily limited to the above-described preferred embodiment, and the above-mentioned scope is not limited to the technical idea of the present invention. It may be embodied in various lyophilizers in a manner different from the examples.

As described above, according to the present invention, the pre-freezing step and the freeze-drying step may be performed in one chamber, thereby providing a freeze-drier that is easy to use.

Therefore, there is an advantage in reducing the manufacturing cost of the lyophilized product by reducing the cost of equipment installation compared to the case of performing the conventional preliminary freeze drying in a separate equipment, there is an advantage that can minimize the installation area.

Claims (10)

An internal space is formed, a chamber 10 having a liquid nitrogen inlet 30 and a nitrogen gas outlet 40 formed therein, an upper vessel 20 installed in the chamber 10, and the vessel 20. Including a passive building injection nozzle (50) for injecting the frozen building within, a heating means (60) for heating the vessel (20), and a vacuum pump (70) for vacuuming the inside of the chamber (10) In the lyophilizer for lyophilizing the liquid frozen dried liquid, Both side walls 11 of the chamber 10 are connected to a motor 82 capable of forward rotation and reverse rotation, and a plurality of rotatable rollers 81 are installed. The upper surface of the container 20 is open, the locking portion 21 is formed to be caught and installed on a plurality of rollers 81 formed in the chamber 10 on both sides of the upper, The liquid nitrogen inlet 30 is formed at one side of the upper wall 12 of the chamber 10 to introduce liquid nitrogen into the container 20, The nitrogen gas outlet 40 is formed on one side of the upper wall 12 in the chamber 10 to discharge nitrogen gas generated by vaporization of liquid nitrogen to the outside, The passive building injection nozzle 50 is formed on one side of the upper wall 12 of the chamber 10 to inject the liquid dry frozen liquid into the container 20 containing the liquid nitrogen, The heating means 60 is disposed below the vessel 20, and the separation distance from the shelf 61 and the shelf 61 and the vessel 20 are installed therein, the pipe 64 for circulating the heat fluid. Lyophilizer, characterized in that consisting of a hydraulic cylinder (63) to adjust. delete The method of claim 1, The inside of the chamber (10) is a lyophilizer, characterized in that formed in the shape of a rectangular parallelepiped. delete delete delete delete The method of claim 1, Freeze-dryer, characterized in that the liquid nitrogen storage tank 31 is installed outside the chamber (10) to supply the liquid nitrogen to the liquid nitrogen inlet (30). The method of claim 1, Freeze-dried dryer, characterized in that the passive dry storage tank 51 is installed on the outside of the chamber (10) for supplying the passive dry to the dried building spray nozzle (50). The method of claim 1, Freeze-dryer, characterized in that the nitrogen gas storage tank 41 is installed on the outside of the chamber 10 to store the nitrogen gas discharged through the nitrogen gas outlet 40.

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