JP5495865B2 - Freeze dryer - Google Patents

Description

  The present invention relates to a freeze dryer, and in particular, a material to be dried adjusted to a liquid state is dispensed into an upright cylindrical tube and frozen on its inner wall surface, and the frozen material to be dried is sublimated under vacuum. It is related with the structure of the dispensing nozzle with which the freeze dryer which obtains dried foodstuffs or chemicals etc. by sublimating water in a material and sublimating moisture in a material is equipped.

  FIG. 4 shows a main part of a freeze dryer previously proposed by the applicant of the present application. As is apparent from this figure, in the freeze dryer of this example, a freeze-drying chamber for the material to be dried is formed by an upright cylindrical tube 101 provided with a jacket 102 for circulating a heat medium on the outer periphery, and the tube The material 120 to be dried supplied from the dispensing nozzle 110 is caused to flow evenly on the inner wall surface 101a of the 101, and the frozen layer A having a uniform thickness is formed on the inner wall surface 101a of the tube 101. ing. Various means can be considered as a means for evenly flowing the material to be dried 120 onto the inner wall surface 101a of the tube 101. In the example of FIG. 4, a funnel-shaped inclined wall 103 is integrally formed on the upper portion of the tube 101. The material to be dried 120 that is formed and sprayed to the inclined surface of the inclined wall 103 in a liquid state from the dispensing nozzle 110 is evenly sprayed, and the material to be dried 120 is applied from the inclined surface of the inclined wall 103 to the inner wall surface 101 a of the tube 101. It is flowing down.

  As shown in FIG. 5, the dispensing nozzle 110 is screwed into a cylindrical dispensing head 111 connected to the supply pipe 130 for the material to be dried 120 and a male screw 111 a formed on the outer peripheral surface of the dispensing head 111. A cylindrical body 112, a bottom plate 113 screwed into a female screw 112a formed inside the body 112, and a packing 114 interposed between the connecting portions of these members 111, 112, 113, The material to be dried 120 is ejected radially from the annular slit 115 formed between the body 112 and the bottom plate 113 in the radial direction of the body 112. Reference numeral 113 a in the drawing denotes a male screw that is erected vertically from the center of one surface of the bottom plate 113 and is screwed into a female screw 112 a formed at the lower part of the inner surface of the body 112. Inside the body 112, a material to be dried distribution plate 112b in which a female screw 112a is formed at the center is provided, and the portion around the material distribution plate 112b to be dried is disposed on the side of the bottom plate 113 from the dispensing head 111 side. A plurality of distribution passages 112c penetrating into the bottom plate 113 are equally divided, and the material 120 to be dried supplied from the pipe 130 is equally distributed in the circumferential direction of the bottom plate 113 (for example, (See Patent Document 1).

  When the dispensing nozzle 110 is used, the liquid material 120 to be dried supplied from the pipe 130 is equally distributed in the circumferential direction of the bottom plate 113 by the plurality of distribution channels 112c opened in the body 112. In addition, the spray amount of the material 120 to be dried sprayed from the annular slit 115 can be equalized in the circumferential direction of the dispensing nozzle 110. Therefore, it is possible to form the frozen layer A having a uniform thickness over the entire inner wall surface 101a of the tube 101, and the sublimation of moisture from the frozen layer A is performed at a uniform speed over the entire surface. A can be lyophilized with high efficiency.

Japanese Patent No. 3866594

  However, since the dispensing nozzle 110 previously proposed by the applicant of the present application is composed of a combination of multiple parts such as the dispensing head 111, the body 112, the bottom plate 113, and the plurality of packings 114 as described above, Contamination and germs are likely to occur at the connecting portions of each member, and it is virtually impossible to ensure contamination hazard prevention and sterilization when freeze-drying foods and chemicals. In addition, if the washing of the dispensing nozzle 110 is repeated frequently, such inconvenience can be avoided to some extent. However, it takes a lot of labor and cost to disassemble and assemble the dispensing nozzle 110 and to wash each part. It is hard to say that it is an effective coping method.

  The present invention has been made to solve such problems of the prior art, and its purpose is to ensure the prevention and sterilization of pollution hazards that are practically sufficient, and maintenance management for pollution prevention. Is to provide a freeze dryer which is easy to handle.

  In order to solve the above problems, the present invention provides a freeze-drying chamber for a material to be dried formed with an upright cylindrical tube, a heat medium circulation jacket disposed on the outer periphery of the tube, In a freeze dryer having a dispensing nozzle that sprays a material to be dried that is adjusted to a liquid state on a wall surface, the dispensing nozzle has a cylindrical portion whose one end is fixed to the tip of the material to be dried supply pipe, A to-be-dried material distribution plate disposed inside the cylindrical portion, one end is connected to the to-be-dried material distribution plate, and a required gap is provided between the to-be-dried material guide surface and the tip end surface of the cylindrical portion. And the orifice portion disposed opposite to each other, and the cylindrical portion, the material to be dried distribution plate, and the orifice portion are inseparably formed.

  Thus, when the dispensing nozzle of the required shape is formed into an integral inseparable shape, unlike the case where the dispensing nozzle is configured from a combination of a plurality of members that can be disassembled, no gap can occur at the connecting portion of each member. Therefore, it is structurally impossible that dirt accumulates in the gap or that germs propagate in the gap, and it is possible to ensure prevention of contamination hazard and sterilization in the dispensing nozzle. This also reduces the frequency of cleaning the dispensing nozzle, and facilitates maintenance management of the dispensing nozzle because it is not necessary to disassemble and reassemble the dispensing nozzle when cleaning the dispensing nozzle. be able to.

  In the freeze dryer having the above-described configuration, the tubular portion and the material to be dried distribution plate are integrated by welding.

  In this way, when the cylindrical portion of the dispensing nozzle and the material to be dried distribution plate are integrated by welding, no gap is generated between these members, and contamination hazards in the dispensing nozzle are prevented and sterilized. Unlike other bonding methods such as adhesion, it is possible to prevent foreign matter from being mixed into the material to be dried.

  According to the present invention, in the freeze dryer having the above-described configuration, the cylindrical portion includes a plurality of portions integrated by welding.

  According to such a configuration, welding of the material to be dried distribution plate to the inner surface of the cylindrical portion can be facilitated, so that the dispensing nozzle can be easily manufactured.

  In the freeze dryer having the above-described configuration, the one end of the cylindrical portion and the tip of the material to be dried supply pipe are integrated by welding.

  According to this configuration, since the dispensing nozzle and the material to be dried supply pipe can be made into one part, the stay of dirt and the propagation of various bacteria can be prevented between the dispensing nozzle and the material to be dried material supply pipe. This can improve the reliability of the freeze dryer.

  According to the present invention, in the freeze dryer having the above-described configuration, the size of the gap formed between the material to be dried guide surface and the tip surface of the cylindrical portion is 0.8 mm or more and 2.0 mm or less. It was configured as follows.

  In order to form a frozen layer with a uniform layer thickness on the inner wall of an upright cylindrical tube that is a freeze-drying chamber for the material to be dried, the material to be dried is formed into a thin film from the entire circumference of the dispensing nozzle. Therefore, it is necessary to inject stably. According to the experiment, by setting the size of the gap formed between the material to be dried formed on the orifice part and the tip surface of the cylindrical part to 0.8 mm or more and 2.0 mm or less, the object to be dried A frozen layer having a uniform layer thickness can be formed on the inner wall surface of the tube under normal injection conditions of the material.

  According to the present invention, in the freeze dryer having the above configuration, the inclination angle of the material to be dried with respect to the central axis of the orifice portion is 30 degrees or more and 60 degrees or less.

  The material to be dried, which is formed into a thin film from the dispensing nozzle and sprayed, collides with the inner wall surface of the tube and flows down from the upper side along the inner wall surface of the tube. And it freezes during the flow and becomes a frozen layer. The inclination angle of the material to be dried with respect to the central axis of the orifice part is related to the number of splashes caused by the liquid film colliding with the inner wall surface of the tube and the particle diameter thereof. If it is large, the uniformity of the thickness of the frozen layer is adversely affected. According to the experiment, by setting the inclination angle of the material to be dried with respect to the central axis of the orifice portion to 30 degrees or more and 60 degrees or less, the layer thickness is uniform on the inner wall surface of the tube under the normal spraying conditions of the material to be dried. A freezing layer can be formed.

  In the freeze dryer having the above-described configuration, the material distribution plate to be dried has a plurality of holes penetrating in a length direction of the cylindrical portion on a circumference centering on a central axis of the orifice portion. It was set as the structure where the distribution flow path was opened equally.

  According to such a configuration, the material to be dried introduced from the pipe into the dispensing nozzle is equally distributed in the circumferential direction of the dispensing nozzle by the plurality of distribution channels established in the material to be dried distribution plate. The material to be dried can be uniformly sprayed from the gap formed between the guide surface of the material to be dried formed in the orifice portion and the tip end surface of the cylindrical portion, and an even layer is formed on the inner wall surface of the tube 1. A thick frozen layer can be formed.

  In the lyophilizer of the present invention, the dispensing nozzle is formed in an inseparable shape with no gap in the connection portion, so that dirt stays in the gap and propagation of germs in the gap cannot occur structurally. Therefore, it is possible to ensure prevention of contamination hazard and sterilization in the dispensing nozzle. In addition, the frequency of cleaning the dispensing nozzle can be reduced, and it is not necessary to disassemble and reassemble the dispensing nozzle when cleaning the dispensing nozzle, thus facilitating maintenance management of the dispensing nozzle. .

It is a block diagram of the freeze dryer which concerns on embodiment. It is sectional drawing of the dispensing nozzle applied to the freeze dryer which concerns on embodiment. It is an end view of the dispensing nozzle applied to the freeze dryer which concerns on embodiment. It is a principal part block diagram of the freeze dryer which concerns on a prior art example. It is sectional drawing of the dispensing nozzle applied to the freeze dryer which concerns on a prior art example.

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

  As shown in FIG. 1, the lyophilizer according to the embodiment has the same configuration as the lyophilizer described in Patent Document 1 with respect to other parts except the dispensing nozzle. That is, a drying cabinet for freeze-drying a liquid material to be dried is formed with an upright cylindrical tube 1, and an outer cylindrical jacket 2 for circulating a heat medium is provided around the tube 1. Is provided. Inside the jacket 2, a plurality of stages (three stages in the example of FIG. 5) of heat medium flow paths 2 a, 2 b, 2 c divided in the length direction of the tube 1 are provided. An inlet pipe 20 and an outlet pipe 21 are provided in each of the heat medium flow paths 2a, 2b, and 2c of each stage, and each of the inlet pipe 20 and the outlet pipe 21 includes a refrigerator d and a heat exchanger. A pipe f of a temperature control device comprising e and a 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, 2c at each stage.

  A dome-shaped duct 3 is provided above the tube 1, and this duct 3 is connected to a vacuum exhaust system (not shown) equipped with a vacuum pump and a cold trap via a valve 30. A pipe 5 extending from a liquid material tank t2 attached to the machine frame F is disposed in the duct 3, and a dispensing nozzle for injecting a liquid material to be dried onto the inner wall surface of the tube 1 is disposed at the tip thereof. 70 is attached. The configuration of the dispensing nozzle 70 will be described later in detail.

  A pipe 90 extending from a distilled water tank t 3 attached to the machine frame F is connected to the pipe 5, and a switching valve V 4 is provided at a junction between the pipe 5 and the pipe 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. In addition, the code | symbol p2 in the figure has shown the feed water pump which supplies the distilled water stored in the distilled water tank t3 to the dispensing nozzle 70 through the conduit | pipe 90, the switching valve V4, and the piping 5. FIG.

  On the other hand, a drying bulk recovery chamber 4 formed in a funnel shape is connected to the lower portion of the tube 1, and this recovery chamber 4 is connected to a pulverizer 8 for finely pulverizing the drying bulk via a transport cylinder 41. A cyclone separator 81 for separating the pulverized material pulverized by the pulverizer 8 into air and powder is connected to the inlet 82, and on the outlet 83 side of the pulverizer 8. The reduced diameter portion of the recovery chamber 4 is provided with a jet nozzle 42 that roughly pulverizes the cylindrical dry bulk recovered from the tube 1 with air pressure. This jet nozzle 42 generates a swirling flow around the axis of the collecting chamber 4 in the collecting chamber 4, and the cylindrical dry bulk that falls from the tube 1 into the collecting chamber 4 by the swirling flow. Coarsely grind. Further, valves V1 and V2 for sequentially discharging the dry bulk coarsely pulverized by the jet nozzle 42 to the pulverizing apparatus 8 side through the conveying cylinder 41 are provided in the small diameter portion of the collection unit 4.

  Further, an extraction pipe 6 provided with a valve V3 is connected between the valve V1 and the valve V2, and the other end of the extraction pipe 6 is connected to a recovery tank t1 for recovering 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 pipe line 6a.

  Hereinafter, the dispensing nozzle 70 according to the embodiment will be described with reference to FIGS. 2 and 3. As is clear from these drawings, the dispensing nozzle 70 according to this embodiment includes a cylindrical portion 71 having one end connected to the pipe 5 and a material distribution plate to be dried disposed inside the cylindrical portion 71. 72 and an orifice part 73 having one end connected to the material distribution plate 72 to be dried.

  The cylindrical portion 71 includes a small-diameter portion 71a connected to the pipe 5, a large-diameter portion 71b to which the material distribution plate 73 to be dried is fixed, and a large-diameter portion that connects the small-diameter portion 71a and the large-diameter portion 71b. 71c. The diameter of the small diameter portion 71 a is determined based on the diameter of the pipe 5, and the diameter of the large diameter portion 71 b is determined based on the diameter of the tube 1. As this cylindrical part 71, the whole thing manufactured as a seamless integrated body can also be used, and what integrated several members by welding can also be used. A cylindrical portion 71 shown in FIG. 2 includes a first member 74 composed of most of the large-diameter portion 71b, a part of the large-diameter portion 71b, a large-diameter portion 71c, and a small-diameter portion 71a. The first part 74 and the second part 75 are integrated by welding. According to such a configuration, before the first part 74 and the second part 75 are welded, the material to be dried material distribution plate 72 is welded to the inner surface of the first part 74, so that the material to be dried material distribution plate 72 with respect to the tubular portion 71 is welded. Therefore, the productivity of the dispensing nozzle 70 can be increased. In addition, since the welding of the 1st component 74 and the 2nd component 75 can form the beautiful weld bead without a welding defect from the front side of a welding part to the back side, it applies full automatic precision welding method called astro welding. Is particularly desirable.

  In addition, although the small diameter part 71a of the dispensing nozzle 70 and the pipe 5 are also connected by welding, it is particularly desirable to apply the astro welding method to the welding of the part for the same reason.

  As shown in FIG. 3, the material distribution plates 72 to be dried are formed in a disk shape, and a plurality (10 in the example of FIG. 3) are arranged on the circumference around the central axis O. The distribution flow path 72a is opened equally. As shown in FIG. 2, the material to be dried distribution plate 72 is welded to the inner surface of the large diameter portion 71 b constituting the cylindrical portion 71. Regarding the welding of the portion, it is particularly desirable to apply the back surface welding method because a uniform corrugated bead can be formed on the back side by one-side welding from the groove side. In addition, the code | symbol W in FIG. 2 has shown each welding part.

  As shown in FIG. 2, the orifice portion 73 includes a columnar connecting portion 73 a connected to the material to be dried distribution plate 72 and a conical body portion 73 b, and It is integrally formed. Therefore, the cylindrical part 71, the material to be dried distribution plate 72, and the orifice part 73 have an integral inseparable structure as a whole. By adopting such a configuration, there is no gap in each connection portion, so there is no structural retention of dirt in the gap and propagation of germs in the gap, and contamination hazards in the dispensing nozzle 70 Prevention and sterilization can be ensured. This also reduces the frequency of cleaning the dispensing nozzle 70 and eliminates the need for disassembling and reassembling the dispensing nozzle 70 when cleaning the dispensing nozzle 70, thus facilitating maintenance management of the dispensing nozzle 70. Can be made.

  As shown in FIG. 2, the conical material to be dried guide surface 72c formed on the main body 72b is disposed opposite to the front end surface of the cylindrical portion 71 with a required gap s therebetween. The It is desirable from the results of various experiments that the gap s between the material to be dried guide surface 72c and the tip surface of the cylindrical portion 71 is 0.8 mm or more and 2.0 mm or less. Further, it is desirable from the results of various experiments that the inclination angle α of the material to be dried guide surface 72c with respect to the central axis OO of the dispensing nozzle 70 is 30 degrees or more and 60 degrees or less.

  Since the dispensing nozzle 70 according to the embodiment has such a configuration, the material to be dried that is formed into a thin film over the entire circumference from between the material guide surface 72c to be dried and the tip surface of the cylindrical portion 71. Can be stably injected. Therefore, a frozen layer having a uniform thickness can be formed on the entire inner wall surface of the tube 1.

  Hereinafter, the operation of the freeze dryer according to the embodiment will be described.

  First, a frozen layer is formed on the inner wall surface of the tube 1. This process is performed by injecting the material to be dried, which is adjusted to be liquid and stored in the liquid material tank t2, from the dispensing nozzle 70 while cooling the tube 1 with the heat medium circulating in the jacket 2. Before the material to be dried is sprayed, the switching valve V4 is switched to the distilled water tank t3 side, and the distilled water supplied from the distilled water tank t3 through the conduit 90 is sprayed from the dispensing nozzle 70. An ice lining layer can also be formed on the inner wall surface. The formation of this ice lining layer is performed to facilitate the removal of the dry bulk from the tube 1, and when the inner wall surface of the tube is highly slippery and the dry bulk can be easily removed. Can be omitted.

  Further, in this frozen layer forming step, heat media adjusted to different temperatures can be circulated through the plurality of stages of jackets 2 arranged along the length direction of the tube 1. For example, when three stages of the heat medium flow paths 2a, 2b, 2c are formed in the jacket 2 along the length direction of the tube 1, the temperature of the heat medium circulating in the upper heat medium flow path 2a So that the temperature of the heat medium circulating in the intermediate heat medium flow path 2b is slightly higher than that, and further, the temperature of the heat medium circulating in the lower heat medium flow path 2c is highest. Moreover, it can adjust with the temperature control apparatus which consists of the refrigerator d, the heat exchanger e, and the heater h. In this way, the material to be dried which is ejected from the dispensing nozzle 70 and flows down the inner wall surface of the tube 1 from above can be quickly frozen above the tube 1. The inconvenience that many tend to freeze can be solved, and a frozen layer having a uniform thickness can be formed on the inner wall surface of the tube 1.

  The liquid material to be dried that has not been frozen on the inner wall surface of the tube 1 and has reached the small diameter portion of the recovery portion 4 is recovered into the recovery tank t1 via the take-out pipe 6. Further, 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 conduit 6a.

  When the frozen layer having a predetermined thickness is formed on the inner wall surface of the tube 1, the spraying of the material to be dried from the dispensing nozzle 70 is stopped, the vacuum exhaust system (not shown) is driven, the valve 30 is opened, The tube 1 and the duct 3 are evacuated to a predetermined degree of vacuum. At this time, the temperature of the heat medium circulating in the jacket 2 is applied to the frozen layer with heat energy corresponding to the sublimation latent heat using a temperature control device including the refrigerator d, the heat exchanger e, and the heater h. Adjust to a possible temperature. Thereby, the frozen layer is freeze-dried, and a dry bulk is generated.

  The dry bulk falls into the collection unit 4 due to its own weight, and is coarsely pulverized by a swirling flow generated by the air pressure injected from the jet nozzle 42. The coarsely pulverized dry bulk is conveyed to the pulverizing device 8 through the conveying cylinder 41 and finely pulverized by a power mill or a jet mill. Further, the finely pulverized dry bulk is conveyed to a cyclone separation device 81 and separated into air and powder. When the dry bulk is easily pulverized and can be finely pulverized by the jet nozzle 42 provided in the collection unit 4, the pulverization by the pulverization device 8 can be omitted.

  In addition, this invention makes the summary the structure of the dispensing nozzle 70, About the structure of another part, it can change suitably irrespective of the said embodiment.

  INDUSTRIAL APPLICABILITY The present invention can be used for a freeze dryer used for freeze drying of foods and medicines.

DESCRIPTION OF SYMBOLS 1 Tube 2 Jacket 2a, 2b, 2c Heat-medium flow path 3 Duct 4 Collection | recovery part 5 Piping 6 Take-out pipe 8 Crushing device 20 Inlet pipe 21 Outlet pipe 30 Valve 41 Transport cylinder 42 Jet nozzle 70 Dispensing nozzle 71 Cylindrical part 71a Small diameter Part 71b large diameter part 71c enlarged diameter part 72 dried material distribution plate 72a distribution flow path 73 orifice part 73a connecting part 73b main body part 73c dried material guide surface 74 first member 75 second member W welded part 81 cyclone separator d Refrigerator e Heat exchanger h Heater f Pipe line t1 Recovery tank t2 Liquid material tank t3 Distilled water tank

Claims (7)

A freeze-drying chamber for a material to be dried formed with an upright cylindrical tube, a jacket for circulating a heat medium disposed on the outer periphery of the tube, and a material to be dried adjusted to a liquid state on the inner wall surface of the tube In a freeze dryer equipped with a dispensing nozzle for spraying,
The dispensing nozzle has a cylindrical portion whose one end is fixed to a tip portion of the material to be dried supplying pipe, a material distribution plate to be dried disposed inside the cylindrical portion, and one end of the material to be dried which distributes the material to be dried. An orifice portion that is connected to the plate and is opposed to the tip portion of the cylindrical portion with a required gap between the guide portion and the cylindrical portion, the material to be dried distribution plate And an lyophilizer characterized in that the orifice part is inseparably formed.   The freeze dryer according to claim 1, wherein the cylindrical portion and the material to be dried distribution plate are integrated by welding.   The freeze dryer according to any one of claims 1 and 2, wherein the cylindrical portion includes a plurality of portions integrated by welding.   The freeze dryer according to any one of claims 1 to 3, wherein one end of the cylindrical portion and a tip of the material to be dried supply pipe are integrated by welding.   The size of the gap formed between the material to be dried guide surface and the tip end surface of the cylindrical portion is 0.8 mm or more and 2.0 mm or less. The freeze dryer according to any one of the above.   The freeze dryer according to any one of claims 1 to 5, wherein an inclination angle of the material to be dried with respect to a central axis of the orifice portion is 30 degrees or more and 60 degrees or less.   In the material to be dried distribution plate, a plurality of distribution passages penetrating in the length direction of the cylindrical portion are equally provided on the circumference centering on the central axis of the orifice portion. The freeze dryer according to any one of claims 1 to 6, characterized in that

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