Vacuum freeze drying equipment and vacuum freeze drying method

Abstract

The present invention provides a vacuum freeze drying device and method capable of continuously performing vacuum freeze drying in a short time; the vacuum freeze drying equipment (1) of the present invention has an exhaust passage for performing vacuum suction, a drying device (3) comprises a tubular portion (31), the tubular portion is tubular and has an inlet portion and an outlet portion, a temperature regulating device (30a-30j) is arranged outside the tubular portion and in a plurality of regions formed from its inlet portion to its outlet portion, the plurality of regions being at least three or more regions whose temperatures can be controlled, and is used to regulate the temperature of a plurality of regions (40a-40j) on the outer surface of the tubular portion (31); a temperature control unit (8) is used to independently control the temperature regulating device; and a rotating portion (7) for rotating the tubular portion (31), the tubular portion (31) having a spiral conveying device (31a) arranged adjacent to its inner wall and continuously arranged from its inlet portion to its outlet portion, and the conveying device (31a) sequentially conveys the frozen material to various positions inside the tubular portion corresponding to the plurality of regions so as to continuously sublimate and dry.

Description

Technical Field

[0001] The invention relates to vacuum freeze drying equipment and a vacuum freeze drying method thereof. Background Art

[0002] Conventionally, Patent Document 1 proposes a freeze-drying device that generates liquid droplets, freezes and solidifies the liquid droplets into frozen particles, and then freeze-dries the frozen particles.

[0003] Furthermore, Patent Document 2 proposes a freeze-drying apparatus in which a shelf for receiving a frozen material is inclined.

[0004] Furthermore, Patent Document 3 proposes a vacuum freeze-drying apparatus in which frozen particles are sublimated and dried using kinetic energy obtained during spraying.

[0005] Prior art literature

[0006] Patent Literature

[0007] Patent Document 1: International Publication No. WO2013 / 050162

[0008] Patent Document 2: International Publication No. WO2010 / 005021

[0009] Patent Document 3: International Publication No. WO2019 / 235036 Summary of the invention

[0010] Problem that the invention aims to solve

[0011] However, there is a problem in the above documents that vacuum freeze drying cannot be performed continuously in a short period of time.

[0012] Therefore, in view of the above problems, the present invention provides a vacuum freeze-drying device and a vacuum freeze-drying method capable of continuously performing vacuum freeze-drying in a short time.

[0013] Solution to the problem

[0014] In order to solve the above problems,

[0015] (1) The present invention provides a vacuum freeze-drying device, comprising a vacuum freezing device for freezing liquid, and a drying device for sublimating and drying the above-mentioned frozen material. The vacuum freeze-drying device also includes an exhaust channel for vacuum suction; the drying device includes: a tubular portion having an inlet and an outlet and being cylindrical; a temperature regulating device arranged outside the tubular portion and in a plurality of regions formed from its inlet to its outlet, wherein the plurality of regions are at least three or more temperature control regions, and the temperature regulating device is used to regulate the temperature of a plurality of regions on the outer surface of the tubular portion; a temperature control unit for independently controlling the temperature regulating device; and a rotating portion for rotating the tubular portion; the tubular portion has a spiral conveying device, which is arranged close to the inner wall of the tubular portion and is continuously arranged from the inlet to the outlet of the tubular portion; the spiral conveying device sequentially conveys the frozen material entering from the inlet to the positions corresponding to the plurality of regions in the tubular portion, so that the frozen material is continuously sublimated and dried.

[0016] (2) In the structural design described in (1) above, the at least three or more regions include at least one negative temperature region, a temperature region from the negative temperature region to the negative temperature region plus 40°C, and a temperature region plus 20°C or higher, which are arranged from the inlet of the tubular portion toward the outlet thereof;

[0017] (3) In the structural design described in (1) or (2) above, the substance produced thereby is an injectable substance or a drug in the form of a solid preparation, and the outside of the tubular portion is covered with clean air.

[0018] (4) In the structural designs described in (1) to (3) above, the rotating part includes a rotational driving force transmission part that transmits the rotational driving force to one or more positions set in the axial direction, and a rotation support part composed of a rotating roller and / or a bearing and set at the rotational driving force transmission part for supporting rotation.

[0019] (5) In the structural designs described in (1) to (4) above, the rotation speed of the rotating part is ≥1 / 30 rpm and ≤1 rpm.

[0020] (6) In the structural designs described in (1) to (5) above, the spiral conveying device is formed by providing a spiral wall on the inner wall of the tubular portion.

[0021] (7) In the structural designs described in (1) to (5) above, the spiral conveying device is formed by opening a groove portion on the inner wall of the tubular portion, and the depth of the groove portion is ≥3 mm and ≤50 mm.

[0022] (8) In the structural designs described in (1) to (7) above, the tubular portion includes a contact or non-contact temperature detection unit; the temperature control unit controls the temperature of the temperature regulating device according to the surface temperature of the tubular portion or the temperature of the material inside the tubular portion detected by the temperature detection unit.

[0023] (9) In the structural designs described in (1) to (8) above, a moisture detection unit is provided on the outside of the tubular portion, which detects the moisture content of the material inside the tubular portion through a transparent glass or resin window, and the temperature control unit controls the temperature of the temperature regulating device according to the moisture content of the material inside the tubular portion detected by the moisture detection unit.

[0024] (10) In the structural designs described in (1) to (9) above, the tubular portion is made of stainless steel.

[0025] (11) The present invention provides a vacuum freeze-drying method, comprising: a vacuum freezing step for freezing liquid; a drying step for sublimating and drying the above-mentioned frozen material; and a step of vacuum suction through an exhaust channel. The drying step comprises: a step of rotating a tubular portion, the tubular portion being in the shape of a tubular body and having an inlet and an outlet, the tubular portion having a spiral conveying device continuously arranged from the inlet to the outlet; a step of adjusting the temperature of a plurality of regions outside the tubular portion and in a direction from the inlet to the outlet, wherein the plurality of regions are at least three or more temperature-controlled regions; and a step of continuously conveying the frozen material to positions corresponding to the plurality of regions in the tubular portion so that the frozen material entering from the inlet is continuously sublimated and dried.

[0026] (12) In the structural designs described in (1) to (10) above, the connecting assembly is composed of a rotatable screw arranged in a conveying pipe, one end of which is arranged at the collecting part of the vacuum freezing device and the other end is arranged in the tubular part; the frozen material entering from the collecting part moves along the axial direction of the screw.

[0027] (13) In the structural design of (12) above, the base end of the screw is supported on one side of the vacuum freezing device through a support portion, and the first suction pipe is arranged on the adjacent side of the support portion, so that the inner cavity of the conveying pipe is always kept in a vacuum state through the first suction pipe; a support portion is provided at the tube end of the conveying pipe located on the drying device side, so that it can be rotatably supported on the tube body end of the tubular body in the drying device; the second suction pipe is arranged between the tube body end of the tubular body and the support portion of the tube end of the conveying pipe, and the inner cavity of the conveying pipe and the inner cavity of the tubular body are always kept in a vacuum state through the second suction pipe.

[0028] (14) In the structural design of (12) or (13) above, the screw is a spiral coil structure arranged around a rotating axis and is disposed close to the inner wall of the conveying tube 55; under the rotation of the screw, the frozen material received by the collecting part is conveyed to the tube body.

[0029] (15) In the structural designs of (12) to (14) above, the rotation drive mechanism for driving the screw to rotate is different from the rotation drive mechanism for driving the tubular portion to rotate.

[0030] Effects of the Invention

[0031] According to the present invention, the vacuum freeze-drying equipment and the vacuum freeze-drying method thereof can continuously perform vacuum freeze-drying in a short time. BRIEF DESCRIPTION OF THE DRAWINGS

[0032] Figure 1 is an explanatory diagram of a vacuum freeze-drying device in an embodiment of the present invention;

[0033] Figure 2 for Figure 1 A cross-sectional view of a drying device, a connecting assembly and a collecting assembly in the vacuum freeze-drying device shown;

[0034] Figure 3 It is a front view of a drying device of a vacuum freeze-drying device in an embodiment of the present invention;

[0035] Figure 4 It is a plan view of the drying device of the vacuum freeze-drying equipment in an embodiment of the present invention.

[0036] Fig. 5 (A) is a left side view of the drying device;

[0037] Fig. 5 (B) is a right side view of the drying device;

[0038] Figure 6 for Figure 1 AA section view;

[0039] Figure 7A to Figure 7E is a schematic structural diagram of a tubular portion 31B among a plurality of tubular body members 31A to 31F constituting the tubular portion;

[0040] Figure 8 A half-section 31BX of the tubular portion 31B;

[0041] Fig. 9 How to detect the temperature of a substance or the humidity inside a substance by a detection unit;

[0042] Fig.10 A cross-sectional view of a connection assembly of a vacuum freeze-drying device according to an embodiment of the present invention;

[0043] Fig.11 for Figure 7A to Figure 7E A schematic structural diagram of a half body 31BX of the middle tubular portion 31B in another embodiment;

[0044] Fig.12 A cross-sectional view of a connecting assembly of a vacuum freeze-drying device according to another embodiment of the present invention. DETAILED DESCRIPTION

[0045] The vacuum freeze drying device according to the embodiment of the present invention will be described below. In addition, the same components or components having the same functions may be represented by the same reference numerals, and in the description, the components that have been described above will be appropriately omitted.

[0046] like Figure 1 FIG. 2 is an explanatory diagram of a vacuum freeze-drying device in an embodiment of the present invention. Figure 2 Shown Figure 2 for Figure 1 A cross-sectional view of a drying device, a connecting assembly and a collecting assembly in a vacuum freeze-drying device is shown.

[0047] exist Figure 1 In the embodiment, the vacuum freeze-drying equipment 1 includes a vacuum freezing device 2, a drying device 3, a connecting component 4 and a collecting component 5.

[0048] The substance processed by the vacuum freeze-drying apparatus 1 is an injectable substance or a drug in a solid preparation.

[0049] For example, the vacuum freezing device 2 sprays a raw material solution containing a raw material from a nozzle 21 into a vacuum container to produce a frozen substance by freezing the sprayed raw material solution. Furthermore, the vacuum freezing device can be a device in which the raw material solution drips from a nozzle into a vacuum container, so that it can produce a frozen substance by freezing the dripping droplets. The sprayed or dripped raw material solution self-freezes during the falling process due to the evaporation of water and the loss of latent heat of evaporation, thereby producing a frozen substance, i.e., a fine frozen particle. The frozen substance falls to a conical collection portion 22 having a smaller opening and is collected by the collection portion 22.

[0050] The connecting assembly 4 connects the vacuum freezing device 2 and the drying device 3 , and is used for transporting the frozen material produced by the vacuum freezing device 2 to the drying device 3 .

[0051] The drying device 3 is used for continuously sublimating and drying the frozen material. The collecting assembly 5 is used for collecting the dry material formed by sublimation and drying in the drying device 3, and the dry material is output from the outlet portion 31c of the tubular portion 31;

[0052] In one embodiment, the vacuum freeze-drying device 1 has an exhaust channel for vacuum suction, wherein the exhaust channel is arranged in the connecting component 4. The exhaust channel can be arranged in the vacuum freezing device 2, the drying device 3 or the connecting component 4. The arrangement of the exhaust channel can maintain the internal reduced pressure atmosphere to form an environment in which liquid is difficult to exist, but solid or gas can exist.

[0053] The tubular portion 31 and the collecting assembly 5 are covered with clean air 6. Any decomposable connection on the tubular portion 31 is covered with clean air 6 so that it is configured to allow clean air to enter to prevent leakage;

[0054] The tubular portion 31 and the collecting assembly 5 are covered by the surrounding clean air 6. The surrounding outer surface portions of any decomposable connection portion on the tubular portion 31 are covered by the clean air 6 so that it is configured to allow the clean air to enter to prevent leakage.

[0055] like Figure 3 The front view of the drying device of the vacuum freeze drying equipment in one embodiment of the present invention is shown. Figure 4 FIG. 5(A) is a plan view of a drying device of a vacuum freeze drying apparatus according to an embodiment of the present invention. FIG. 5(B) is a left view of the drying device, and FIG. 5(A) is a right view of the drying device. Figure 6 Shown Figure 1 AA section view;

[0056] like Figures 1 to 6 As shown, the drying device 3 includes a tubular portion 31 , a temperature adjustment device 30 a - 30 j , a rotating portion 7 and a temperature control unit 8 .

[0057] The tubular portion 31 is a tubular body having an opening and extending linearly in the horizontal direction, and has an inlet portion 31b for allowing the frozen substance to enter, and an outlet portion 31c for allowing the sublimated and dried dry substance to be sent out (see Figure 2 ).

[0058] In the tubular portion 31, the spiral conveying device 31a is continuously arranged from the inlet portion 31b to the outlet portion 31c adjacent to the inner wall of the tubular portion 31. The frozen material transported by the connecting assembly 4 enters from the inlet portion 31b of the tubular portion 31 and is transferred to the outlet portion 31c through the spiral conveying device 31a, during which the frozen material is continuously sublimated and dried.

[0059] The temperature adjustment devices 30 a - 30 j are provided outside the tubular portion 31 to adjust the temperatures of a plurality of regions 40 a - 40 j on the outer surface of the tubular portion 31 .

[0060] The temperatures of the plurality of regions 40a to 40j from the inlet 31b to the outlet 31 of the tubular portion 31 can be independently controlled. The temperature adjustment devices 30a to 30j adjust the temperatures of the plurality of regions 40a to 40j to adjust the temperatures of the respective locations in the tubular portion 31 corresponding to the plurality of regions 40a to 40j.

[0061] In this embodiment, there are ten temperature adjustment devices 30a-30j, so the multiple regions are formed by the temperature adjustment devices 30a-30j. The multiple regions 40a-40j preferably include at least 3 or more regions. It should be noted that the multiple temperature adjustment devices can be collectively referred to as a temperature adjustment device, or each temperature adjustment device can also be described as each temperature adjustment device.

[0062] The rotating part 7 is used to rotate the tubular part 31 along its center line. When the rotating part 7 drives the tubular member 31 to rotate, the frozen material is sequentially transferred from the inlet part 31b of the tubular member 31 to the outlet part 31c of the tubular member 31 through the spiral conveying device 31a. In this process, the frozen material is continuously sublimated and dried. The rotating part 7 only drives the tubular part 31 to rotate, and does not drive the temperature adjustment devices 30a to 30j outside the tubular part 31 to rotate. The temperature adjustment devices 30a to 30j are all fixed and do not rotate.

[0063] The temperature control unit 8 has a function of inputting and outputting information, and can independently control the temperature adjustment devices 30 a to 30 j to adjust the temperatures of the plurality of areas 40 a to 40 j formed outside the tubular portion 31 .

[0064] Next, the temperature adjustment methods 30a to 30j will be described.

[0065] like Figure 1 and Figure 2 As shown, the temperature adjustment devices 30a~30j can independently adjust the temperature of the outer space around the tubular portion 31 and adjust the temperature of each space in the tubular portion 31 respectively.

[0066] The temperature adjustment device 30a adjusts the spatial temperature of the region 40a and adjusts the temperature of the internal space of the tubular portion 31 corresponding to the region 40a. In addition, the temperature adjustment device 30b adjusts the spatial temperature of the region 40b and adjusts the temperature of the internal space of the tubular portion 31 corresponding to the region 40b. The temperature adjustment device 30c adjusts the spatial temperature of the region 40c and adjusts the temperature of the internal space of the tubular portion 31 corresponding to the region 40c. Similarly, the temperature adjustment devices 30d to 30j adjust the spatial temperature of the regions 40d to 40j and adjust the temperature of the internal space of the tubular portion 31 corresponding to the regions 40d to 40j, respectively.

[0067] The frozen material entering from the inlet portion 31b of the tubular portion 31 is continuously sublimated and dried through the spaces regulated by the temperature regulating devices 30a to 30j.

[0068] Next, refer to Figure 3 to Figure 6The temperature adjustment devices 30a to 30j are described in detail in conjunction with an embodiment. Although the temperature adjustment device 30b is described as an example in this embodiment, other temperature adjustment devices can be arranged in a similar manner.

[0069] The temperature regulating device 30b includes a wall portion 32 disposed on one side of the inlet portion 31b of the tubular portion 31, a wall portion 33 disposed on one side of the outlet portion 31c, a cover body 34 for covering the space surrounded by the walls 32 and 33, and a duct 35a and a duct 35b for supplying air to the wall 32 or 33, respectively. The walls 32 and 33 are both circular. The cover body 34 is made of a material such as a transparent resin so that the inside thereof can be visualized, and it is also used to cover the space surrounded by the walls 32 and 33. The walls 32 and 33 are connected to the ducts 35a and 35b so that the ducts 35a and 35b can supply air. The temperatures of the plurality of regions 40a to 40j are adjusted to each target temperature by supplying air in this manner.

[0070] An air blowing device (not shown) is connected to the duct 35a and the duct 35b and provides temperature control gas. By supplying the gas from the duct 35a and the duct 35b to the areas 40a to 40j covered by the wall 32, the wall 33 and the cover body 34, the temperatures of the plurality of areas 40a to 40j are independently controlled. For example, air may be supplied as the gas, but it is not limited to air.

[0071] Although the temperature adjustment devices 30a to 30j are described by taking gas as an example, they are not limited to gas, and electric heaters, refrigerants, etc. may also be used.

[0072] The inner sides of the wall portions 32, 33 have circular openings matching the outer shape of the tubular portion 31. The inner openings of the wall portions 32, 33 are preferably close to the outer circumference of the tubular portion 31.

[0073] Next, the temperatures of the plurality of regions 40 a to 40 j will be described.

[0074] The plurality of regions 40a-40j are at least three or more regions from the inlet 31b to the outlet 31c of the tubular portion 31, and these three or more regions include the following temperature regions (1)-(3). The temperature regions are defined by measuring the temperature of the tubular portion 31 (i.e., the tube body itself) when the process reaches a stable operating state, and measuring the outer surface temperature of the tubular portion 31 in a contact and / or non-contact manner.

[0075] The temperature region includes at least (1) a negative temperature region, (2) a temperature region from the negative temperature region to the negative temperature region plus 40°C, and (3) a temperature region plus 20°C or higher.

[0076] Negative temperature area (1) refers to an area with negative temperature, such as -40℃, -30℃, -20℃, etc.

[0077] The temperature region (2) from the negative temperature region to the negative temperature region plus 40°C refers to the temperature region formed from the negative temperature of the negative temperature region (1) to the negative temperature plus 40°C. For example, when the temperature of the negative temperature region (1) is -40°C, based on -40°C plus 40°C, the temperature region (2) becomes a temperature region of -40°C to 0°C. In addition, when the temperature of the negative temperature region (1) is -20°C, based on -20°C plus 40°C, the temperature region (2) becomes a temperature region of -20°C to 20°C.

[0078] The temperature zone (3) of plus 20°C or higher means that when the upper limit temperature of the temperature zone (2) is 0°C, the temperature range is 0°C + 20°C and above.

[0079] The multiple regions 40a~40j from the inlet portion 31b to the outlet portion 31c of the tubular portion 31 include at least the above-mentioned three regions (1)~(3). The spiral conveying device 31a sequentially conveys the frozen material or the dry material to the corresponding positions of the multiple regions 40a~40j in the tubular portion 31 corresponding to the above-mentioned temperature regions (1)~(3), so that the frozen material or the dry material is continuously sublimated and dried.

[0080] Next, the tubular portion 31 will be described.

[0081] The tubular portion 31 is preferably made of stainless steel. The length of the tubular portion 31 is between 100 mm and 2000 mm, preferably between 150 mm and 1000 mm, and more preferably between 200 mm and 500 mm.

[0082] The tubular portion 31 is a tubular body formed by a plurality of tubular bodies 31A to 31F and connectors 31G to 31K connected in sequence. The tubular portion 31 may also be a tubular body that does not require connectors. The tubular bodies 31B, 31C, 31D, and 31E are formed by tubular bodies having the same shape. The tubular body 31A is a tubular body having a slightly shorter length. The tubular body 31F is a tubular body whose cross-sectional shape becomes smaller toward the end. The connectors 31G to 31K are tightly connected between the connected tubular bodies to prevent them from falling off.

[0083] As described above, the tubular portion 31 is provided with a spiral conveyor 31a, which is arranged near the inner wall of the tubular portion 31 and is continuously arranged from its inlet portion 31b to its outlet portion 31c. The spiral conveyor 31a can be formed into a spiral structure by providing a wall portion or a groove on the inner periphery of the tubular portion 31. The method of forming the spiral structure also includes a method of embedding a screw into the inner periphery of the tubular portion 31.

[0084] The spiral conveyor 31a conveys the frozen material entering from the inlet 31b to the inner cavity of the tubular portion 31 corresponding to the plurality of regions 40a to 40j in sequence to continuously sublimate and dry the frozen material, and conveys the sublimated and dried dry material to the outlet 31c.

[0085] Next, the structure of the rotating portion will be described.

[0086] like Figure 3 to Figure 6 As shown, the rotating portion 7 includes a motor 71 , pulleys 72 , 73 , a belt 74 , rotating shafts 75 , 76 , and rotating rollers 77 , 78 .

[0087] The motor 71 is a rotation drive source. The pulleys 72, 73, the belt 74 and the rotating shafts 75, 76 are rotation drive transmission parts for transmitting the rotation drive. The rotating rollers 77, 78 are rotation support parts for supporting the rotation of the rotation drive transmission parts. The rotation support parts can be configured by adding bearings to the rotating rollers 77, 78, or the rotating roller 77 can be replaced by bearings.

[0088] The belt 74 is hung on the pulleys 72 and 73. The rotational driving force of the motor 71 is transmitted through the conveyor belt 74. Rotating rollers 77 are arranged on both sides below the tubular portion 31. The tubular portion 31 is placed on the rotating rollers 77 arranged on both sides.

[0089] The pulley 73 is connected to one end of the rotating shaft 75. The rotating roller 78 is connected to a fixed base in the pulley 73, and similarly, the rotating roller 78 connected to the fixed base is also provided at the other end of the rotating shaft 75. Eight rotating rollers 77 are connected to the rotating shaft 75 between the rotating rollers 78 and 78 located on both sides.

[0090] One end of the rotating shaft 76 is connected to a fixed base of a rotating roller 78 on one side, and the other end is connected to a fixed base of the rotating roller 78. Between the two rotating rollers 78 and 78, eight rotating rollers 77 are connected to the rotating shaft 76. The rotating roller 77 connected to the rotating shaft 75 is a driving roller, and the rotating roller 77 connected to the rotating shaft 76 is a driven roller.

[0091] When the motor 71 rotates, the belt 74 rotates via the pulley 72 , the rotating shaft 75 rotates by the rotation of the pulley 73 , and the tubular portion 31 rotates by the rotation of the rotating roller 77 fixed to the rotating shaft 75 , and the rotating roller 77 rotates as a driven roller connected to the rotating shaft 76 .

[0092] Next, the rotation speed of the tubular portion 31 will be described.

[0093] The tubular portion 31 is preferably rotated by the rotating portion 7 at a rotation speed of ≥1 / 30 rpm and ≤1 rpm.

[0094] Next, the temperature detection unit and the humidity detection unit are described.

[0095] like Figure 3 and Figure 4 As shown, in the tubular portion 31, glass windows (window portions) 36 are continuously arranged at certain intervals along the circumferential direction, and the glass windows 36 are arranged at multiple positions (in this embodiment, at eight positions) along the longitudinal direction of the tubular member 31. The arrangement of the glass windows 36 can realize the state of the internal substance to be identified and detected from the outside. The glass windows 36 can be made of resin.

[0096] The detection unit 37 is arranged at the lower side of the tubular portion 31, wherein the glass window 36 is arranged along the circumferential direction. The detection unit 37 includes at least three types, and includes a temperature detection unit for detecting the temperature of the substance inside the tubular portion 31, a temperature detection unit for detecting the temperature of the outer surface (wall surface) of the tubular portion 31, and a moisture detection unit for detecting the moisture content of the substance inside the tubular portion 31.

[0097] When the detection unit 37 is used as a temperature detection unit to detect the temperature of the substance in the tubular portion 31, it can be configured as a contact type or a non-contact type. When the detection unit 37 used as the temperature detection unit is a contact type, it detects the surface temperature of the tubular portion 31. When the detection unit 37 used as the temperature detection unit is a non-contact type, it detects the temperature of the substance inside the tubular portion 31 through the glass window 36 on the tubular portion 31.

[0098] The temperature control unit 8 can independently control the temperatures of the temperature adjustment devices 30 a to 30 j according to the surface temperature of the tubular portion 31 or the temperature of the substance inside the tubular portion 31 detected by the detection unit 37 through the glass window 36 .

[0099] In addition, when the detection unit 37 is used as a moisture detection unit and is used to detect the moisture content of the substance in the tubular portion 31, it can detect the moisture content of the substance in the tubular portion 31 through the transparent glass window 36. The temperature control unit 8 can independently control the temperature of the temperature adjustment devices 30a to 30j according to the moisture content of the substance inside the tubular portion detected by the detection unit 37.

[0100] like Fig. 9 It shows how the detection unit detects the temperature of a substance or the amount of water inside the substance.

[0101] like Fig. 9 As shown, when the detection unit 37 is used as a temperature detection unit for detecting the temperature of the material inside the tubular portion 31 and a moisture detection unit for detecting the moisture content of the material inside the tubular portion 31, it can detect the temperature of the material X inside the tubular portion 31 and the moisture of the material inside the tubular portion through the transparent glass window 36 on the tubular portion 31.

[0102] The detection unit 37 can detect the temperature of the substance X in the tubular portion 31 and the humidity of the substance in the tubular portion 31 through each transparent glass window 36 arranged at a certain interval along the circumferential direction of the tubular portion 31. In addition, since the glass windows 36 and the detection unit 37 are arranged at multiple positions in the longitudinal direction of the tubular portion 31, the temperature and moisture content of the substance can be accurately detected at each position of the tubular portion 31.

[0103] Next, the screw conveying device 31a will be described.

[0104] like Figure 7A to Figure 7E The tube body 31B is shown among the multiple tube bodies 31A to 31F constituting the tubular portion 31. Fig. 7A As shown Figure 3 A perspective view of the tube body 31B is shown, Figure 7B Shown is a front view of the tube body 31B, as shown in Figure 7C FIG. 31B is a side view of the tube body 31B. Fig.7D FIG. 3 is a cross-sectional view of the tube body 31B. Fig. 7E Shown Fig.7D This is an enlarged view of part B. Figure 8 Shown is a half body 31BX of the tubular body 31B.

[0105] In addition, in Figures 7 and Figure 8 In the figure, the glass window 36 is omitted because the spiral conveyor 31a is located at Figure 3 The center of the middle tube 31B.

[0106] As shown in Figs. 7 and 8, the tubular body 31B constituting the tubular portion 31 is tubular in shape, and has edge portions 31d protruding radially at both open ends thereof. The tubular portion 31 is formed by fixing the edge portions 31d of adjacent tubular bodies among 31A to 31F to each other. The edge portions 31d of adjacent tubular bodies among 31A to 31F are fixed to each other by connecting ferrules, clamping or bolting.

[0107] The screw conveyor 31a portion is formed continuously from one end to the other end of the tube body 31B.

[0108] like Fig. 7E As shown, as a part of the spiral conveying device 31a, a wall portion is continuously formed on the inner wall of the half body 31BX of the tube body, such as the wall portion 31a1 in the first circle and the wall portion 31a2 in the second circle, and thus a part of the spiral conveying device 31a can be formed in the half body 31BX of the tube body.

[0109] The height of the wall portion 31a1 and the wall portion 31a2 is the height of the screw conveyor 31a, and is preferably set within a range of ≥3 mm and ≤50 mm, for example.

[0110] like Figure 8 The half body 31BX of the tubular body 31B is shown, and one tubular body 31B is formed by combining two half bodies 31BX. When the tubular body 31B is combined with the screw conveying device 31a, the half body 31BX of the tubular body 31B can form the tubular body 31B having part of the screw conveying device 31a.

[0111] like Fig.10 Shown is a cross-sectional view of the connection assembly of the vacuum freeze-drying equipment in this embodiment.

[0112] like Fig.10 As shown, the connection assembly 4 is arranged between the collecting portion 22 of the vacuum freezing device 2 and the end of the inlet portion 31b of the drying device 3, and is used to transport the frozen material produced by the vacuum freezing device 2 to the drying device 3. A receiving port 302 is provided at the end 301 for receiving the frozen material transported by the connection assembly 4.

[0113] The connection assembly 4 includes an inner tube 41, an outer tube 42, a screw 43 disposed in the inner tube 41, and an intermediate tube 44 extending from the end 301 of the drying device 3 to between the inner tube 41 and the outer tube 42 of the connection assembly 4. A bearing 45 and an air seal 46 are disposed between the outer tube 42 and the intermediate tube 44 and on one side of the drying device 3.

[0114] The air seal 46 is used to seal the rotating shaft by supplying air from the flow path without contacting the rotating shaft.

[0115] like Fig.11 Shown Figure 7A to Figure 7E A schematic structural diagram of a half body 31BX of the middle tubular portion 31B in another embodiment.

[0116] As shown in Figure 7 and Figure 8 In the embodiment shown, the wall portion on the inner wall of the tubular portion 31 forms a spiral conveying device 31a. Fig.11 As shown, grooves 131a1, 131a2, ... may also be formed on the inner wall of the tubular portion 31 to form a conveying device 131a.

[0117] The tube body 31B can be formed into one tube body 31B by connecting two halves 131BX of the tube body. When the two halves 131BX of the tube body 31B are connected, the groove parts constituting the spiral transmission mode 131a are respectively continuously formed. The depth of the groove part 131a1 and the groove part 131a2 is the depth of the transmission device 131a, and is preferably set in the range of ≥3mm and ≤50mm, for example. The spacing between the groove part 131a1 and the groove part 131a2 is the spacing of the transmission device 131a, and is preferably set in the range of ≥5mm and ≤20mm, for example.

[0118] The conveying device 131a forms a spiral groove portion in the inner circumferential surface of the tubular portion 31 around the rotation axis to give a spiral feeding action to the inside of the tubular portion 31, thereby being able to continuously convey frozen substances or dry substances.

[0119] According to this embodiment, a vacuum freeze-drying device and a vacuum freeze-drying method thereof which can continuously perform vacuum freeze-drying in a short time can also be provided.

[0120] In this embodiment, the vacuum freeze drying method includes: a vacuum freezing step of the frozen liquid; a drying step of sublimating and drying the frozen material; and a vacuum suction step through the exhaust channel. The drying step includes: a step of rotating the tubular portion 31, the tubular portion 31 is in the shape of a tube body and has an inlet portion 31b and an outlet portion 31c, and the tubular portion 31 has a spiral conveying device 31a continuously arranged from the inlet portion 31b of the tubular portion to its outlet portion 31c; a step for adjusting the temperature of multiple areas outside the tubular portion 31 and from its inlet portion 31b to its outlet portion 31c, wherein the multiple areas are at least three or more temperature control areas; and a step in which the frozen material is continuously conveyed to the tubular portion 31 and at positions corresponding to the multiple areas so that the frozen material entering from the inlet portion 31b is continuously sublimated and dried.

[0121] Next, refer to Fig.12 Another structure of the connection component is described. Fig.12 It is a cross-sectional view of a connecting component 4B of a vacuum freeze-drying device according to another embodiment of the present invention.

[0122] First, in the vacuum freeze-drying apparatus, a connection assembly 4B for transferring the frozen material from the vacuum freezer 2 to the drying device 3 is provided between the vacuum freezer 2 for freezing liquid and the drying device 3 for sublimating and drying the frozen material. The structure of the connection assembly 4B is designed as follows: the frozen material moves through the screw 58 provided in the transfer pipe 55, and the transfer pipe 55 is connected to the collecting part 22 of the vacuum freezer 2 in the axial direction. However, the transfer direction of the screw 43 to transfer the frozen material to the tubular part 31 is not necessarily in the horizontal direction.

[0123] The base end (left end) of the screw 58 is supported by a support portion 56 (here, a bearing), and the first suction pipe 53 is provided adjacent to the support portion, and is provided so as to maintain a constant vacuum state (high vacuum is sufficient) inside the delivery pipe 55. The first suction pipe 53 is connected to a vacuum pump, but its illustration and description are omitted.

[0124] A support portion 51 is provided at one end of the conveying pipe 55, and the support portion is rotatably supported on an end member 52 of the tube body 31A on the tubular portion 31 of the drying device. A second suction pipe 54 is provided toward the end member 52, and its port is located between the end member 52 and the support portion 51, so that the inside of the conveying pipe 55 and the inside of the tubular portion 31 are both kept in vacuum. The suction port 54 is connected to a vacuum pump, but its illustration and description are omitted.

[0125] The screw 58 is a spiral coil structure arranged around the rotating shaft 57 and is arranged close to the inner wall of the conveying tube 55. The screw 58 delivers the frozen material received from the collecting part 22 into the tubular part 31 by rotating. The coil structure can be a spiral structure or a structure in which the fragments form a coil. In short, it is a structure that can exhibit a continuous feeding function. The above-mentioned setting close to each other is to provide a gap between the coil structure and the conveying tube 55 so that the frozen material will not be stuck and damaged.

[0126] The motor 60 for driving and the coupling 59 for transmitting the driving force of the motor 60 to the rotating shaft 57 are installed at one end of the rotating shaft 57, and the end is opposite to the tubular portion 31. As described above, the motor 60 and the motor 71 are used to rotate the driving screw 58 and the rotating driving tubular portion 31, respectively, so that the conveying state of the frozen material to the drying device 3 can be arbitrarily changed, for example, the speed of the motor 60 is increased to increase the conveying amount. In addition, in the connection component 4 (see Fig.10 ) in the embodiment, the end of the screw 43 on one side of the drying device 3 must be mechanically connected to the tube body 31A of the tubular portion 31, so the structure of the boundary portion between the connecting component 4 and the tubular portion 31 becomes complicated; although in another form of connecting component 4B, the end of the screw 58 extends into the tubular portion 31, which has the advantage of effectively transporting the frozen material.

[0127] Although the above embodiments describe the present invention, it should be noted that the technical scope of the present invention is not limited to the scope of the above embodiments, and it is clear to those skilled in the art that various modifications or improvements may be made to the above embodiments. In addition, it is clear from the description of the scope of the claims that the form in which such modifications or improvements are added may be included in the technical scope of the present invention.

[0128] Figure ID

[0129] 1. Vacuum freeze drying equipment

[0130] 2. Vacuum freezing device

[0131] 3. Drying equipment

[0132] 4. Connect components

[0133] 4B. Connecting components

[0134] 6. Clean air

[0135] 7. Rotating part

[0136] 8. Temperature control unit

[0137] 30a~30j, temperature regulating device

[0138] 31. Tubular part

[0139] 31a. Screw conveyor

[0140] 36. Glass window (window)

[0141] 37. Detection unit (temperature detection part, moisture detection part)

[0142] 40a~40j, multiple areas

[0143] 46. ​​Air seal.

Claims

1. A vacuum freeze drying device, include ： A vacuum freezing device for freezing liquid, and a drying device for sublimating and drying the frozen substance frozen as above, The vacuum freeze-drying device includes an exhaust passage for performing vacuum suction to produce a reduced pressure atmosphere inside the vacuum freezing device and the drying device; Wherein, the drying device comprises: A tubular portion formed by a tubular body having an inlet portion and an outlet portion; A temperature regulating device is arranged outside the tubular portion and in a plurality of regions formed from its inlet to its outlet, wherein the plurality of regions are at least three or more temperature control regions, and the temperature regulating device is used to regulate the temperature of the plurality of regions on the outer surface of the tubular portion; A temperature control unit for independently controlling the temperature regulating device; and a rotating portion for rotating the tubular portion; The tubular portion has a spiral conveying device, which is arranged near the inner wall of the tubular portion and is continuously arranged from the inlet to the outlet of the tubular portion; the spiral conveying device is continuously formed in the tubular body (31B) from one end to the other end; a wall portion is continuously formed on the inner wall of a half body (31BX) of the tubular body, and a tubular body (31B) is formed by combining two half bodies (31BX); when the tubular body (31B) is combined with the spiral conveying device (31a), the half body (31BX) of the tubular body (31B) can form a tubular body (31B) having a part of the spiral conveying device (31a); The vacuum freeze-drying device comprises a connecting assembly for connecting a vacuum freezing device and a drying device, wherein the connecting assembly comprises a first tube body arranged on one side of the vacuum freezing device, a second tube body arranged on one side of the drying device, and a tubular portion for rotation as described above is arranged therein, and a sealing member arranged between the first tube body and the second tube body and used for sealing; The tubular portion includes a plurality of tube bodies and a connecting piece for connecting the plurality of tube bodies; The temperature regulating device is provided in each temperature zone, and includes a first wall portion, a second wall portion, a cover body covering the space surrounded by the first wall portion and the second wall portion to form a zone, and a supply device for supplying gas into the zone, and is surrounded by the cover body, and in a state where the inside of the vacuum freezing device and the drying device is a reduced pressure atmosphere, the rotating portion rotates the tubular portion, so that the spiral conveying device sequentially conveys the frozen material entering from the vacuum freezing device to the positions in the tubular portion corresponding to the plurality of zones, so as to continuously sublimate and dry the frozen material; The at least three or more regions include at least one negative temperature region arranged from the inlet of the tubular portion toward the outlet thereof, a temperature region from the negative temperature region to the negative temperature region plus 40°C, and a temperature region plus 20°C or higher.

2. The vacuum freeze-drying equipment according to claim 1, characterized in that: The substance is an injectable substance or a drug in the form of a solid preparation, and the outside of the tubular portion is covered with clean air.

3. The vacuum freeze-drying device according to claim 1 or 2, characterized in that: The rotating portion includes a rotational driving force transmitting portion that transmits a rotational driving force to one or more positions provided in the axial direction, and a rotation supporting portion that is composed of a rotation roller and / or a bearing and is provided at the rotational driving force transmitting portion for supporting rotation.

4. The vacuum freeze-drying device according to claim 1 or 2, characterized in that: The rotation speed of the rotating part is ≥1 / 30rpm and ≤1rpm.

5. The vacuum freeze-drying equipment according to claim 1 or 2, characterized in that: The spiral conveyor is formed by providing a spiral wall on the inner wall of the tubular portion.

6. The vacuum freeze-drying equipment according to claim 1 or 2, characterized in that: The spiral conveying device is formed by opening a groove portion on the inner wall of the tubular portion, and the depth of the groove portion is ≥3mm and ≤50mm.

7. The vacuum freeze-drying equipment according to claim 1 or 2, characterized in that: The tubular portion includes a contact or non-contact temperature detection unit; The temperature control unit controls the temperature of the temperature adjustment device according to the surface temperature of the tubular portion or the temperature of the substance inside the tubular portion detected by the temperature detection unit.

8. The vacuum freeze-drying equipment according to claim 1 or 2, characterized in that: A moisture detection unit is provided on the outside of the tubular portion, which detects the moisture content of the substance inside the tubular portion through a transparent glass or resin window; The temperature control unit controls the temperature of the temperature adjustment device according to the moisture content of the material inside the tubular portion detected by the moisture detection unit.

9. The vacuum freeze-drying equipment according to claim 1 or 2, characterized in that: The tubular portion is made of stainless steel.

10. The vacuum freeze-drying equipment according to claim 1, characterized in that: The connecting assembly is composed of a rotatable screw arranged in a conveying pipe, one end of which is arranged at the collecting part of the vacuum freezing device and the other end is arranged in the tubular part; the frozen material entering from the collecting part moves along the axial direction of the screw.

11. The vacuum freeze-drying equipment according to claim 10, characterized in that: The base end of the screw is supported on one side of the vacuum freezing device through a support portion, and a first suction pipe is arranged on the adjacent side of the support portion, so that the inner cavity of the conveying pipe is always kept in a vacuum state through the first suction pipe; a support portion is provided at the tube end of the conveying pipe located on the drying device side, so that it can be rotatably supported on the tube body end of the tubular body in the drying device; the second suction pipe is arranged between the tube body end of the tubular body and the support portion of the tube end of the conveying pipe, and the inner cavity of the conveying pipe and the inner cavity of the tubular body are always kept in a vacuum state through the second suction pipe.

12. The vacuum freeze-drying equipment according to claim 10 or 11, characterized in that: The screw is a spiral coil structure arranged around a rotating axis and is disposed close to the inner wall of the conveying tube; when the screw rotates, the frozen material received by the collecting part is conveyed into the tube body.

13. The vacuum freeze-drying equipment according to claim 10 or 11, characterized in that: The rotation drive mechanism for driving the screw to rotate is different from the rotation drive mechanism for driving the tubular portion to rotate.

14. A vacuum freeze-drying method using the vacuum freeze-drying device according to claim 1, characterized in that: include: Steps for vacuum freezing the frozen liquid, a drying step of sublimating and drying the frozen substance, and A step of performing vacuum suction through the exhaust passage to create a reduced pressure atmosphere inside the vacuum freezing device and the drying device; The connecting assembly is used to connect the vacuum freezing device and the drying device. The drying steps include: The step of rotating the tubular portion, wherein the tubular portion is in the shape of a tube and has an inlet portion and an outlet portion, and the tubular portion has a spiral conveying device continuously arranged from the inlet portion to the outlet portion of the tubular portion, A step for adjusting the temperature of a plurality of zones outside the tubular portion and in a direction from its inlet portion to its outlet portion, wherein the plurality of zones are at least three or more temperature-controlled zones, and By rotating the tubular portion in a vacuum freezing device and a drying device in a state of reduced pressure atmosphere, the frozen material entering from the inlet portion is continuously transferred to positions in the tubular portion corresponding to multiple areas, so as to continuously perform sublimation and drying steps.

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