WO2017084162A1 - 一种全自动密闭式喷雾冻干生产设备及方法 - Google Patents

一种全自动密闭式喷雾冻干生产设备及方法 Download PDF

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Publication number
WO2017084162A1
WO2017084162A1 PCT/CN2015/098807 CN2015098807W WO2017084162A1 WO 2017084162 A1 WO2017084162 A1 WO 2017084162A1 CN 2015098807 W CN2015098807 W CN 2015098807W WO 2017084162 A1 WO2017084162 A1 WO 2017084162A1
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Prior art keywords
spray
vacuum
freeze
drying
drum
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PCT/CN2015/098807
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English (en)
French (fr)
Inventor
郑效东
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上海东富龙科技股份有限公司
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    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F26—DRYING
    • F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
    • F26B5/00—Drying solid materials or objects by processes not involving the application of heat
    • F26B5/04—Drying solid materials or objects by processes not involving the application of heat by evaporation or sublimation of moisture under reduced pressure, e.g. in a vacuum
    • F26B5/06—Drying solid materials or objects by processes not involving the application of heat by evaporation or sublimation of moisture under reduced pressure, e.g. in a vacuum the process involving freezing
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F26—DRYING
    • F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
    • F26B11/00—Machines or apparatus for drying solid materials or objects with movement which is non-progressive
    • F26B11/02—Machines or apparatus for drying solid materials or objects with movement which is non-progressive in moving drums or other mainly-closed receptacles
    • F26B11/04—Machines or apparatus for drying solid materials or objects with movement which is non-progressive in moving drums or other mainly-closed receptacles rotating about a horizontal or slightly-inclined axis

Definitions

  • the invention relates to a fully automatic closed spray freeze-drying production equipment, which is used in a pharmaceutical freeze-drying workshop, and belongs to the technical field of vacuum freeze-drying.
  • Vacuum freeze drying also known as sublimation drying.
  • the principle is to freeze the solution to be lyophilized in a closed environment, and then give a certain temperature and vacuum to remove the moisture in the frozen solution by sublimation.
  • freeze-drying technique can be used in the following fields: production of foods and microorganisms, production of medicines represented by injection medicines, production and processing of blood products, and manufacture and processing of various other materials.
  • the liquid A to be lyophilized needs to be pre-filled into a container B such as a glass bottle or a tray, and the container B is placed on the flat layer C to be frozen.
  • a container B such as a glass bottle or a tray
  • the temperature of the plate is heated in a vacuum environment to heat the ice, and the water vapor sublimates and leaves a dry substance.
  • the material to be dried is always allowed to stand, and only a small area of the bottom is in contact with the plate layer, and heat transfer is limited, especially when the material is pre-loaded into a container of a poorly-conducted conductor such as a glass bottle for lyophilization.
  • the heat effect is poor, and the drying time is long; the upper surface of the static material is first dried, and the dry layer gradually descends toward the frozen layer. At this stage, the dry layer becomes a hindrance to the outward diffusion of the sublimated water vapor of the frozen layer, and the mass transfer effect is poor.
  • the drying time is further extended; in addition, static drying imposes high requirements on the uniformity of the sheet temperature.
  • US Patent Publication No. US20130118026A1 discloses a spray lyophilization technique in which a liquid to be lyophilized is sprayed from a nozzle above a container, and another set of nozzles sprays liquid nitrogen, which is in contact with the refrigerant during the falling of the lyophilized droplet.
  • Heat exchange quick freezing forms ice particles; ice particles are placed in a conical container, and are rotated by a stirrer to heat the material through the cone wall; the stirrer flips to apply mechanical force to the material, and the friction and collision effects easily destroy the original shape of the material. State; and the material must be piled up to a certain height in the cone to be flipped by the agitator. This accumulation also hinders the bottom sublimation water vapor from spreading outward; in addition, the conical dryer can only be dried in several stages.
  • Another quick-freezing technique is to place liquid nitrogen at the bottom of the container, and the lyophilized liquid is sprayed or dripped from above, and is frozen through the low temperature zone of liquid nitrogen.
  • Freeze-drying processes are widely used in, but not limited to, the pharmaceutical industry, and their products have stringent requirements for clean, sterile pharmaceutical processes.
  • the above two quick freezing technologies use the refrigerant (liquid nitrogen) to directly contact the material for refrigeration. The cleanliness and sterility are difficult to ensure, and the refrigerant is vaporized after heat exchange. Re-formation of the liquid requires great energy, and direct discharge is easy to cause. Waste and pollution.
  • the technical problem to be solved by the present invention is to provide a method for improving the freezing and drying efficiency of a liquid to be lyophilized in a freeze-drying process, while maintaining the original shape state of the material after freezing, protecting the cleanliness and sterility of the product, and allowing the freezing Dry continuous spray freeze-drying production equipment to shorten freeze-drying cycle, increase production efficiency, reduce the risk of drug contamination, reduce cost and energy consumption.
  • the technical proposal of the present invention is to provide a fully automatic closed spray freeze-drying production equipment, which comprises: a vacuum spray freezing granulation device and a dynamic heating drying device which are connected to each other to form a closed container;
  • the vacuum spray freezing granulation device comprises a spray canister provided with an atomizing nozzle for atomizing and dispersing a liquid to be lyophilized into droplets, the spray canister connection for forming a vacuum in a closed container
  • the environment causes a part of the droplets to vaporize and absorb heat in the vacuum environment to cool the droplets to a frozen shape.
  • a vacuum system for ice particles for ice particles.
  • some of the components of the droplets are water.
  • the droplets are not in direct contact with the refrigerant in the closed container.
  • the spray can is part of a closed container, the upper portion being cylindrical and the lower portion being tapered.
  • the atomizing nozzle is connected to a closed liquid distribution pipe, and the liquid distribution pipe is provided with a flow regulating device.
  • the vacuum spray freeze granulation device further comprises a condensing device for condensing a portion of the vaporized droplets.
  • the condensing device is one of a first cooling jacket and a condenser, and the first cooling jacket is disposed outside the upper portion of the spray cylinder, and the first cooling jacket is internally connected.
  • the condenser is disposed outside the spray can and is connected to the spray can.
  • the vacuum system comprises a vacuum pump
  • the spray cylinder is provided with a connection port, and a valve is arranged on the connection port;
  • the condensation device is a first refrigeration jacket
  • the vacuum pump is connected to the connection port of the spray can by a pipe;
  • the condensing device is a condenser or a combination of a first cooling jacket and a condenser
  • the condenser is connected to the connection port of the spray can by a pipe, and the vacuum pump is connected to the condenser through another pipe.
  • a filter net is disposed on the connection port of the spray can.
  • the refrigerant in the first refrigeration jacket forms a circulation through a fluid pump on the pipeline and is cooled by the heat exchanger.
  • the first refrigerating jacket has a rectangular cross section and is disposed in a circle around the upper portion of the spray cylinder; or the first refrigerating jacket has a semicircular cross section and is spirally surrounded.
  • the refrigerant in the first refrigeration jacket may be silicone oil.
  • the refrigerant temperature is -40 ° C to -100 ° C.
  • the lower tapered outer side of the spray can is provided with a second cooling jacket for preventing the ice particles from melting, and the second cooling jacket is provided with a refrigerant.
  • the refrigerant in the second refrigeration jacket forms a circulation through a fluid pump on the pipeline and is cooled by the heat exchanger.
  • the second cooling jacket has a rectangular cross section and is arranged in a circle around the outer side of the cone; or the second cooling jacket has a semicircular cross section and spirally surrounds the outer side of the cone
  • the refrigerant in the second cooling jacket may be silicone oil.
  • the temperature of the refrigerant in the second cooling jacket is -10 ° C to -40 ° C.
  • the bottom of the spray can is provided with a discharge tube for discharging ice particles.
  • the outer wall of the spray can, the upper side wall and the outer side of the tapered side wall are provided with at least one vibrator for shaking ice particles into the lowering tube.
  • the discharge tube is connected to the dynamic heating and drying device, and the connected pipe has a valve.
  • the dynamic heating and drying device comprises an outer cylinder; a rotary dryer portion for accommodating and heating the material is disposed in the outer cylinder; and a temperature control circulation system for controlling the heating temperature of the rotary dryer is connected to the rotary dryer.
  • the outer cylinder is a part of a closed container, and the outer cylinder is provided with
  • a feed pipe for connecting a discharge tube of a vacuum spray freeze granulation device
  • the spray can of the vacuum spray freeze granulation device is connected to the outer cylinder of the dynamic heat drying device to form a complete closed container.
  • the vacuum discharge mechanism is used for discharging the dry material from the vacuum sealed container, returning to atmospheric pressure to dispense the collection tank or connecting to other receiving devices, the mechanism being driven by the upper discharge valve, the buffer Zone, re-pressure pipe, suction pipe and lower discharge valve.
  • an upper discharge valve and a lower discharge valve are disposed below the discharge port of the dynamic heating and drying device, and a buffer area is disposed between the upper discharge valve and the lower discharge valve, and the buffer area is provided with an exhaust valve.
  • the pipeline is connected to the outer cylinder of the dynamic heating and drying device, and the buffer zone is also connected with a dry clean sterile gas inlet pipe provided with a pressure-reducing valve; the receiving device is connected with the lower discharge valve.
  • the rotary dryer comprises
  • a motor used to power the rotation of a shaft.
  • all of the drum and a part of the rotating shaft are disposed in the closed container, and another part of the rotating shaft is connected to the motor outside the sealed container.
  • rotating shaft and the outer cylinder are connected by a shaft seat.
  • At least one hollow jacket is disposed outside the drum, and the fluid in the hollow jacket causes the wall to heat up or cool down.
  • the hollow jacket has a rectangular cross-sectional shape and is arranged around the outer circumference of the rotating cylinder; the hollow jacket is one or more segments arranged in a straight line along the center line of rotation; each hollow jacket is provided
  • the fluid enters and exits the pipeline, and the internal fluid circulation causes the cylinder wall to heat up or cool down.
  • the inner wall of the rotating drum is provided with at least one guiding groove at an angle to the rotation center line of the rotating drum.
  • the material is guided by the guiding groove to migrate toward the discharging port; when the rotating drum rotates in the opposite direction The material is brought back.
  • the temperature control circulation system comprises a rotary joint, a heat exchanger, an electric heater and a fluid pump which are sequentially connected to form a closed loop, and the circulating fluid is closed in the closed loop.
  • the rotary joint is a device for one-side fixed connection, one side for connecting the rotary body and continuously conveying the fluid in any continuous or discontinuous rotational movement of the rotary body, and continuously delivering current.
  • the rotating shaft is internally provided with a passage for fluid circulation, and one side of the passage is connected to one or more hollow jackets on the rotating drum in the outer cylinder container; the other side of the passage is outside
  • the outside of the canister is connected to the rotary joint.
  • the rotary joint causes the fluid in the closed circuit to be continuously conveyed within the hollow jacket during any rotationally continuous or discontinuous rotational movement of the rotary shaft.
  • the fluid is water or silicone oil.
  • a detector for detecting material information is provided in the rotating drum, the information may be temperature; a detector is connected to the rotary joint; and the rotary joint rotates in any continuous or discontinuous rotational motion of the rotating shaft. The current is delivered without interruption.
  • the fully automatic closed spray lyophilization production device further comprises a cleaning and sterilizing system for introducing clean water into the closed container for cleaning, and introducing the disinfectant into the closed container for sterilization.
  • the disinfectant may be none. Pure steam of bacteria.
  • the fully automatic closed spray freeze-drying production apparatus further comprises a control system for automatically controlling the program of the vacuum spray freeze granulation and the dynamic heat drying process, the control system comprising a programmable logic controller ( At least one of a PLC) and a computer (PC).
  • a programmable logic controller At least one of a PLC
  • PC computer
  • the invention also provides a fully automatic closed spray freeze-drying production method, which adopts the above-mentioned fully automatic closed spray freeze-drying production equipment, and the steps are as follows:
  • Step 1 selectively opening or closing each valve of the device, and using a vacuum system to draw the closed container to a certain degree of vacuum;
  • Step 2 atomizing and dispersing the liquid to be lyophilized into droplets by using an atomizing nozzle, and spraying the droplets into the spray cylinder, and some components in the droplets vaporize and absorb heat in a vacuum environment to lower the droplet temperature.
  • the condensing device condenses a portion of the vaporized droplets to maintain a degree of vacuum in the container, and the droplet temperature continues to decrease until freezing forms ice particles;
  • Step 3 adding the ice granule material into the rotating drum through the feeding pipe; the temperature of the rotating drum is controlled by the temperature control circulating system; the rotating drum continuously rotates during the drying process, and the material is tumbling at the bottom of the rotating drum to fully and uniformly contact the cylinder wall
  • the guide groove rotates with the drum to bring the material from the bottom of the drum, and the material slides on the guide groove in the direction of the discharge port due to gravity.
  • the guide groove continues to rotate with the drum, the material falls to the bottom of the rotary tube due to gravity;
  • the amount of spray and the rotation speed of the drum the material migrates to the discharge port at an appropriate rate and evenly spreads on the bottom of the drum without forming a pile.
  • the sublimation gas is quickly discharged from the surface of the material and the gap of the particles and is evacuated and condensed by the vacuum system.
  • the material On the surface of the condensing device; the material is continuously tumbling through the rotating drum and gradually moving forward, and gradually drying in the drum until it is completely dry;
  • Step 4 The dry material falls from the drum into the discharge port; when the material needs to be discharged, the upper discharge valve is opened, the material falls into the buffer area, the upper discharge valve and the suction valve are closed; the re-pressure valve is opened, and the buffer is opened.
  • the area is cleaned and cleaned with sterile gas, so that the pressure difference between the buffer area and the receiving device is the same; the lower discharge valve is opened, the dry material is collected by the receiving device, and the material in the buffer area is drained, and the lower discharge valve and the double pressure valve are closed. , open the suction valve and replace the receiving device; repeat this step when you need to discharge again.
  • the present invention has the following beneficial effects:
  • the liquid is frozen into granules by vacuum spray freezing granulation technology, which greatly improves the freezing rate of the liquid to be lyophilized.
  • the contact between the refrigerant and the material completely eliminates the risk of contamination of the material, improves the sterility of the freeze-drying process, reduces the energy consumption of the production, and the refrigerant is recycled, and does not pollute the environmental discharge.
  • the lyophilized material is dynamically tumbling in the rotating drum through the rotary dryer, fully and uniformly heated, and the sublimation gas is quickly discharged, thereby improving the drying efficiency and shortening the drying time of the material; the material mainly relies on itself in the heating and drying device. Gravity is tumbling or migrating, the original physical state is protected; and the drying process can be carried out continuously.
  • the material after lyophilization is transferred from the vacuum closed loop to the normal pressure through the vacuum discharge mechanism to ensure that the freeze-drying process can be carried out continuously, and the sealed container is protected from environmental pollution.
  • the equipment in the whole freeze-drying production system is kept closed, and the liquid to be lyophilized is added to the dry granules for release. All feeding, freeze-drying and discharging processes are carried out in a sterile and closed environment, which reduces the risk of materials being polluted by the environment or polluting the environment; and the whole process can be carried out continuously to ensure the tightness and sterility of the freeze-drying process. And continuity.
  • Figure 1 is a schematic view showing the structure of a conventional freeze-drying apparatus
  • Embodiment 2 is a schematic structural view of a fully automatic closed spray freeze-drying production apparatus provided in Embodiment 1;
  • Figure 3 is a schematic view showing the structure of a vacuum spray freezing granulation apparatus in Embodiment 1;
  • Embodiment 4 is a schematic structural view of a dynamic heating and drying device in Embodiment 1;
  • Figure 5 is a schematic structural view of a vacuum discharge mechanism in Embodiment 1;
  • FIG. 6 is a schematic structural view of a fully automatic closed spray freeze-drying production apparatus provided in Embodiment 2;
  • Figure 7 is a schematic structural view of a vacuum spray freezing granulation apparatus in Embodiment 2.
  • Embodiment 8 is a schematic structural view of a fully automatic closed spray freeze-drying production apparatus provided in Embodiment 3;
  • Figure 9 is a schematic view showing the structure of a vacuum spray freezing granulation apparatus in Embodiment 3.
  • Figure 10 is a schematic view showing the structure of a dynamic heating and drying device in Embodiment 4.
  • FIG. 2 is a schematic structural view of a fully automatic sealed spray freeze-drying production apparatus provided by the embodiment, wherein the apparatus comprises a vacuum spray freeze granulation device sequentially connected to form a closed container, and a dynamic heating and drying device.
  • FIG. 3 is a schematic structural view of a vacuum spray freeze granulation apparatus 1 provided in the embodiment, the apparatus comprising a spray cylinder 1-1 for accommodating products in a spray granulation process; and a plurality of liquids for lyophilizing Atomizing nozzle 1-2 that is atomized and dispersed into droplets and sprayed into the spray can 1-1; for forming a vacuum environment in the closed container to vaporize a part of the droplets in the vacuum environment The heat further reduces the temperature of the droplets by freezing to form a vacuum system of ice particles; and a condensing means for condensing a portion of the vaporized droplets.
  • the atomizing nozzle 1-2 is disposed in the spray can 1-1.
  • the vacuum system is connected to the spray can 1-1.
  • the upper portion of the spray can 1-1 is cylindrical and the lower portion is tapered.
  • the condensing device is a first cooling jacket 1-3 that is provided with a refrigerant on the outer side of the upper portion of the spray cylinder 1-1, and the refrigerant is silicone oil.
  • the silicone oil is circulated through the fluid pumps 1-4 on the pipe and cooled by the heat exchanger 1-5.
  • the first cooling jacket 1-3 has a rectangular cross section and is disposed in a circle around the upper portion of the spray cylinder 1-1.
  • the lower tapered outer side of the spray can 1-1 is provided with a second cooling jacket 1-6 for preventing the ice particles from melting, and the refrigerant introduced therein is silicone oil.
  • the silicone oil is circulated through the fluid pumps 1-4 on the other set of tubes and cooled by the heat exchanger 1-5.
  • the second cooling jacket 1-6 has a rectangular cross section and is disposed around the outer circumference of the lower portion of the spray cylinder 1-1.
  • the two heat exchangers 1-5 are connected to the refrigeration system 1-7.
  • the refrigeration system 1-7 is a compressor.
  • the atomizing nozzle 1-2 is connected to the closed liquid distribution pipe 1-8, and the liquid to be lyophilized is introduced into the pipe, and the flow regulating pipe 1-9 is provided on the liquid distribution pipe 1-8.
  • the vacuum system includes a vacuum pump 1-10 connected to the spray can 1-1 via conduits 1-11, and the conduits 1-11 are provided with valves 1-12.
  • a filter 1-13 is provided on the connection port of the spray can 1-1.
  • the bottom of the spray can 1-1 is provided with a discharge valve 1-14 for discharging ice particles, and the outer side of the top wall, the upper side wall and the lower side wall of the spray can 1-1 is provided with one for ice Vibrators with particle sag 1-15.
  • the vibrators 1-15 are driven to vibrate by a motor.
  • the discharge valve 1-14 is connected to the dynamic heating and drying device through a pipe.
  • FIG. 4 is a schematic structural view of a dynamic heating and drying device 2 according to the embodiment, the device includes: an outer tube 2-1, a feeding tube 2-2, a discharging port 2-4, and a discharge port having a valve;
  • the spray cylinder 1-1 is connected to the feed pipe 2-2 through the discharge valve 1-14, and the spray cylinder 1-1 and the outer cylinder 2-1 form a closed container and protect the material in the container from environmental pollution or pollute the environment;
  • the motor 2-13 rotational power is transmitted to the drum 2-11; a temperature control circulation system consisting of the rotary joint 2-21, the heat exchanger 2-22, the electric heater 2-23, and the fluid pump 2-24.
  • At least one hollow jacket 2-15 is disposed outside the drum 2-11, and each hollow jacket 2-15 is connected to the inner passage of the shaft 2-12 through a pipe, and all of the drum 2-11, the shaft 2 - A portion of 12 is mounted in a closed container; another portion of the shaft 2-12 is coupled to the motor 2-13 outside the hermetic container, and the internal passage of the portion is coupled to the rotary joint 2-21; the rotary joint 2-21 is One side is used for the fixed connection, and the other side is for connecting the rotating shaft 2-12 and continuously transporting the fluid in any of its rotationally continuous or discontinuous rotational movements, continuously delivering the current.
  • the fluid introduced into the temperature control circulation system is silicone oil, and the silicone oil is heated by the electric heaters 2-23 and adjusted by the heat exchanger 2-22 and circulated through the fluid pumps 2-24 to make the hollow jacket 2-15
  • the wall of the tube is warmed or cooled.
  • FIG. 5 is a schematic structural diagram of a vacuum discharge mechanism 3 according to the embodiment, wherein the mechanism includes an upper discharge valve 3-1, a lower discharge valve 3-2, and two under the discharge port 2-4.
  • the buffer zone 3-3 between the discharge valves, the buffer zone 3-3 is connected to the closed container through the pipeline with the suction valve 3-5, and the buffer zone 3-3 is also connected with the pressure regulating valve 3-6.
  • a line for drying clean sterile gas is introduced; the receiving tank 3-4 is connected to the lower discharge valve 3-2.
  • the sealed container of the device may also be provided with clean water for container cleaning, and a disinfectant may be introduced for sterilization of the container, and the disinfectant is preferably sterile steam.
  • the liquid to be lyophilized may be a normal temperature aqueous solution, a suspension, an emulsion, etc., with or without excipients, to dissolve 125 g of ivy powder in 2 L of water.
  • An example of an aqueous solution of ivy powder includes the following steps:
  • Step 1 First, the sealed container composed of the spray can 1-1 and the outer cylinder 2-1 is evacuated to a vacuum by a vacuum system, and the degree of vacuum is 300 Pa.
  • Step 2 The temperature of the first cooling jacket 1-3 is controlled to be -60 ° C, and the temperature of the second cooling jacket 1-6 is controlled to -20 ° C; the aqueous solution of the ivy powder is passed through the liquid distribution pipe 1-8 It is sent to the atomizing nozzle 1-2, the spray pressure is 0.4 MPa, the nozzle diameter is 1.0 mm, and the liquid is atomized and dispersed into droplets by the atomizing nozzle 1-2 and sprayed into the spray cylinder 1-1, the water in the droplet After vaporization in a vacuum environment, the heat is absorbed to lower the temperature of the droplet, and the vacuum system continues to evacuate.
  • the first cooling jacket 1-3 condenses the vaporized water on the inner wall of the spray cylinder 1-1 to maintain the vacuum.
  • the dropping temperature continues to decrease until freezing forms ice particles, and the process is completed in only a few seconds, and the ice particles are shaken to the bottom of the spray can 1-1 by the vibration of the vibrators 1-15.
  • the droplets are frozen in the spray can 1-1 without being in direct contact with the refrigerant.
  • Step 3 The ice particles of the material are added to the drum 2-11 through the feed pipe 2-2.
  • the hollow jacket 2-15 of the rotating drum 2-11 is controlled by the temperature control circulation system to have a heating temperature of 20 ° C; the drum 2-11 is continuously rotated during the drying process, and the material is tumbling at the bottom of the drum, fully evenly The contact with the cylinder wall is heated; the guiding groove 2-14 rotates with the rotating drum to bring the material from the bottom of the rotating drum, and the material slides on the guiding groove by gravity to the direction of the discharging opening 2-4, and the guiding groove continues to rotate with the rotating drum. The material is dropped by gravity to the bottom of the rotary cylinder.
  • the material migrates to the discharge port at an appropriate rate and evenly spreads at the bottom of the rotating drum without forming a stack; sublimation gas Quickly discharged from the surface of the material and the gap between the particles through the vacuum system and condensed on the inner wall of the upper part of the spray can 1-1; the material is continuously tumbling through the rotating drum and gradually moving to the discharge port, and gradually drying in the drum. Until completely dry.
  • Step 4 The dry material falls from the drum 2-11 into the discharge port 2-4; when the material needs to be discharged, the upper discharge valve 3-1 is opened, the material falls into the buffer zone 3-3, and the material is closed.
  • the fully automatic closed spray freeze-drying production equipment is automatically controlled by a control system composed of a programmable logic controller and a computer during the freeze-drying process.
  • Embodiment 6 is a schematic structural view of a fully automatic sealed spray freeze-drying production apparatus provided in Embodiment 2. This embodiment differs from Embodiment 1 in a vacuum spray freeze granulation apparatus section.
  • FIG. 7 it is a schematic structural view of a vacuum spray freeze granulation apparatus in Embodiment 2, which is similar to Embodiment 1, except that the condensing device is disposed outside and connected to the spray can 1-1.
  • Condenser 1-30 the condenser 1-30 is connected to the connection port of the spray can 1-1 through a pipe 1-11, and the vacuum pump 1-10 is connected to the condenser 1-30 through another pipe, the condenser A valve 1-12 is disposed on the connecting pipe 1-11 of the spray cylinder 1-1, and the first cooling jacket 1-3 is not disposed on the outer side of the upper portion of the spray cylinder 1-1.
  • Step 2 During the liquid quick freezing process, the liquid droplets are sprayed into the spray cylinder 1-1, the water is vaporized in a vacuum environment, the heat is absorbed to lower the temperature of the liquid droplets, the vacuum system is continuously evacuated, and the condenser 1-30 is vaporized. After the water Condensation further maintains the degree of vacuum within the vessel, and the droplet temperature continues to decrease until freezing forms ice particles.
  • Step 3 The sublimation gas is discharged during the heating and drying process, and is evacuated by a vacuum system and condensed on the condenser 1-30.
  • Embodiment 8 is a schematic structural view of a fully automatic sealed spray freeze-drying production apparatus provided in Embodiment 3. This embodiment differs from Embodiment 1 in a vacuum spray freeze granulation apparatus portion.
  • FIG. 9 it is a schematic structural view of a vacuum spray freezing granulation apparatus in Embodiment 3, which is similar to Embodiment 1, except that the condensing device is a first cooling jacket 1-3 and a condenser. a combination of 1-30, the first refrigeration jacket 1-3 is disposed outside the upper portion of the spray cylinder 1-1, and the condenser 1-30 is disposed outside the spray cylinder 1-1; the condenser 1-30 is connected to the connection port of the spray can 1-1 through the pipe 1-11, and the vacuum pump 1-10 is connected to the condenser 1-30 through another pipe, and the connection pipe of the condenser 1-30 and the spray can 1-1 Valves 1-12 are provided on 1-11.
  • the condensing device is a first cooling jacket 1-3 and a condenser. a combination of 1-30, the first refrigeration jacket 1-3 is disposed outside the upper portion of the spray cylinder 1-1, and the condenser 1-30 is disposed outside the spray cylinder 1-1; the condens
  • Step 2 During the liquid quick freezing process, the liquid droplets are sprayed into the spray cylinder 1-1, the water is vaporized in a vacuum environment, and the heat is absorbed to lower the temperature of the liquid droplets, and the vacuum system continues to evacuate, the first refrigeration jacket 1 - 3 The vaporized water is condensed on the inner wall of the spray can 1-1, and the condenser 1-30 condenses the vaporized water, thereby maintaining the vacuum inside the container, and the droplet temperature continues to decrease until freezing forms particles.
  • Step 3 The sublimated gas is discharged during the heating and drying process, and is evacuated by a vacuum system and condensed on the upper inner wall of the spray can 1-1 and the condenser 1-30.
  • the spray can 1-1 of the vacuum spray freeze granulation apparatus provided in this embodiment is externally connected to a plurality of condensers 1-30, and the apparatus is continuously subjected to spray freeze-drying production.
  • Embodiment 2 is a schematic structural view of a fully automatic sealed spray freeze-drying production apparatus provided in Embodiment 4.
  • the structure of this embodiment can be the same as Embodiments 1, 2, and 3, and the implementation steps are different.
  • Step 2 The liquid droplets are sprayed into the spray cylinder 1-1 during the quick freezing process, and the spray is stopped after freezing to form a certain batch of ice particles.
  • Step 3 The material frozen into ice particles is fed into the drum 2-11 through the feed pipe 2-2.
  • the drum 2-11 rotates, and the material rolls at the bottom of the drum.
  • the temperature control circulation system does not heat the hollow jacket 2-15; after the feeding is completed, the temperature control circulation system starts to heat, and the drum 2-11 passes the motor 2
  • the 13 drive is rotated for a period of time, it is reversed. After several rotation directions, the material gradually migrates to the left and right in the drum until the material added is completely dry.
  • Step 4 When the material needs to be discharged, the re-pressure valve 3-6 of the vacuum discharge mechanism and the suction valve 3-5 are sequentially opened, and the dry clean sterile gas is introduced into the buffer zone 3-3 and the closed container to make the container
  • the pressure is consistent with the pressure difference of the receiving device 3-4, and the upper discharge valve 3-1 and the lower discharge valve 3-2 are opened, so that the discharge port 2-4 is connected to the receiving device 3-4, and the rotating cylinder 2 11 Continuous forward until the material is empty.
  • This embodiment uses a freeze-dried production material of a batch of fully automatic closed spray freeze-drying production equipment.

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Abstract

一种全自动密闭式喷雾冻干生产设备及方法，其中生产设备包括真空喷雾冷冻造粒装置（1）和动态加热干燥装置（2）和将干燥物料从真空密闭容器放出的真空出料机构（3）。真空喷雾冷冻造粒装置（1）包括喷雾筒（1-1）、设置在喷雾筒（1-1）内用于将待冻干液体雾化分散为液滴的雾化喷嘴（1-2）和与喷雾筒（1-1）连接的用于在密闭容器中形成真空环境使液滴中的部分组分在真空环境中气化吸热进而使液滴冻结形成颗粒的真空系统。动态加热干燥装置（2）包括组成密闭容器的外筒（2-1）、容纳并加热干燥物料的回转干燥器。回转干燥器部分设于密闭容器内，加热循环系统用于控制回转干燥器温度。喷雾冻干过程在密闭条件下进行，不使用冷媒与物料接触，降低了药品污染的风险，保证了喷雾冻干生产的密闭性、无菌性和连续性。

Description

一种全自动密闭式喷雾冻干生产设备及方法 技术领域
本发明涉及一种全自动密闭式喷雾冻干生产设备，用于药厂无菌冻干车间，属于真空冷冻干燥技术领域。
背景技术
真空冷冻干燥，也称升华干燥。其原理是在密闭环境中将待冻干的溶液进行冷冻，然后给予一定的温度和真空度，使被冻结的溶液中的水分通过升华的方式去除。
真空冷冻干燥有如下的优点：
(1)低温下冻干药品不会导致药品变性或发生活性损失。
(2)在冻干的药品中，微生物的生长和酶的催化作用几乎是不可能发生的。
(3)通过冻干，药品可以非常好的保持初始的体积和形状。
(4)药品中容易被氧化的成分可以很容易的被保护。
(5)利于长期保存。
(6)大部分冻干药品可以在室温下进行储存。
基于上述优点，冷冻干燥技术可以用于以下领域：食品和微生物的生产，以注射剂原料药为代表的药品的生产，血液制品的生产加工，以及各种其它材料的制造和加工。
传统的冷冻干燥工艺中，如图1所示，需要将待冻干的液体A预先灌装入玻璃瓶或托盘等容器B中，再将该容器B盛放在平面放置的板层C上冻结成冰，真空环境下板层升温对冰块加热，水蒸气升华并留下干燥物质。此干燥过程中，待干燥物料始终是静置的，只有底部小范围区域与板层接触，传热有限，特别是当物料预先装入玻璃瓶等热不良导体的容器中进行冻干时，传热效果差，干燥时间长；静置的物料上表面最先干燥，干燥层逐渐向冻结层下降，在这一阶段，干燥层成为冻结层升华水蒸气向外扩散的阻碍，传质效果差，进一步延长了干燥时间；此外，静置干燥对板层温度均匀性也提出了很高的要求。
公开号为US20130118026A1的美国专利公开了一种喷雾冻干技术，其是将待冻干液体从容器上方用喷嘴喷下，另一组喷嘴喷射液氮，待冻干液滴下落过程中与冷媒接触换热，速冻形成冰颗粒；冰颗粒置于锥形容器中，使用搅拌器翻动，通过锥壁加热干燥物料；搅拌器翻动对物料施加机械力，其摩擦、碰撞作用容易破坏物料原有的形体状态；而且物料在锥体内必须堆积到一定高度方能被搅拌器翻动，这种堆积也阻碍底部升华水蒸气向外扩散；此外，锥形干燥器只能分次进行干燥。
另有一种速冻技术是将液氮置于容器底部，待冻干液体从上方喷下或滴下，穿过液氮低温区进行速冻。冷冻干燥工艺被广泛应用在(但不限于)制药工业中，其制品对洁净的、无菌的制药工艺有着严格要求。以上两种速冻技术都使用冷媒(液氮)与物料直接接触制冷，其洁净度、无菌性难以保证，并且冷媒换热后汽化，重新制成液态需消耗极大能量，直接排放则容易造成浪费和污染。
综上所述，如何提高冷冻干燥工艺中待冻干物料的冷冻及干燥效率，并且该过程应尽量避免破坏物料原有的形体状态；更重要的是如何在冻干工艺中保护物料的洁净度与无菌性，避免物料在设备之间输送受环境污染或污染环境；更进一步地使冷冻干燥连续进行，同时降低能耗，均成为了本领域技术人员亟待解决的问题。
发明内容
本发明要解决的技术问题是提供一种能够提高冷冻干燥工艺中待冻干液体的冷冻及干燥效率，同时保持物料冷冻后原有的形体状态，保护制品的洁净度与无菌性，使冷冻干燥连续进行的喷雾冻干生产设备，以缩短冻干周期、提高生产效率、降低药品受污染的风险、降低成本和能耗。
为解决上述技术问题，本发明的技术方案是提供一种全自动密闭式喷雾冻干生产设备，其特征在于：包括互相连接组成密闭容器的真空喷雾冷冻造粒装置和动态加热干燥装置；
所述的真空喷雾冷冻造粒装置包括喷雾筒，所述喷雾筒内设有用于将待冻干液体雾化分散为液滴的雾化喷嘴，所述喷雾筒连接用于在密闭容器中形成真空环境使所述的液滴中的部分组分在该真空环境中汽化吸热进而使液滴降温冻结形 成冰颗粒的真空系统。
优选地，所述液滴中的部分组分为水。
优选地，所述液滴在密闭容器内不与冷媒直接接触。
优选地，所述喷雾筒为密闭容器的一部分，上部为筒形，下部为锥形。
优选地，所述雾化喷嘴连接密闭的配液管道，所述配液管道上设有流量调节装置。
优选地，所述真空喷雾冷冻造粒装置还包括用于将汽化后的所述液滴中的部分组分冷凝的冷凝装置。
更优选地，所述冷凝装置为第一制冷夹套和冷凝器中的一种或其组合，所述的第一制冷夹套设于所述喷雾筒上部的外侧，第一制冷夹套内部通有冷媒；所述冷凝器设于所述的喷雾筒外，并与所述喷雾筒连接。
优选地，所述真空系统包括真空泵，所述的喷雾筒设有连接口，连接口上设有阀门；当所述的冷凝装置为第一制冷夹套时，真空泵通过管道连接喷雾筒的连接口；当所述的冷凝装置为冷凝器或第一制冷夹套和冷凝器的组合时，冷凝器通过管道连接喷雾筒的连接口，真空泵通过另一管道连接冷凝器。
进一步地，所述喷雾筒的连接口上设有过滤网。
进一步地，所述第一制冷夹套内的冷媒通过管道上的流体泵形成循环并通过热交换器降温。
进一步地，所述第一制冷夹套的截面为矩形，以环绕所述喷雾筒的上部一圈的形式设置；或者，所述第一制冷夹套的截面为半圆形，以螺旋状环绕所述喷雾筒的上部若干圈的形式设置，所述的第一制冷夹套内的冷媒可以是硅油。
进一步地，所述的冷媒温度为-40℃～-100℃。
优选地，所述喷雾筒的下部锥形外侧设有用于避免冰颗粒融化的第二制冷夹套，第二制冷夹套内通有冷媒。
进一步地，所述第二制冷夹套内的冷媒通过管道上的流体泵形成循环并通过热交换器降温。
进一步地，所述第二制冷夹套的截面为矩形，以环绕锥形外侧一圈的形式设置；或者，所述的第二制冷夹套的截面为半圆形，以螺旋状环绕锥形外侧若干圈的形式设置，所述的第二制冷夹套内的冷媒可以是硅油。
进一步地，所述的第二制冷夹套内的冷媒温度为-10℃～-40℃。
优选地，所述喷雾筒底部设有用于放出冰颗粒的下料管。
更优选地，所述喷雾筒的顶壁、上部侧壁和锥形侧壁的外侧设有至少一个用于把冰颗粒震落到下料管内的振动器。
更优选地，所述的下料管与所述的动态加热干燥装置相连接，且相连接的管道上有阀门。
所述的动态加热干燥装置包括外筒；用于容纳并加热物料的回转干燥器部分设于外筒内；用于控制回转干燥器加热温度的控温循环系统与回转干燥器连接。
优选地，所述外筒为密闭容器的一部分，外筒上设有
用于连接真空喷雾冷冻造粒装置下料管的进料管；
及用于放出干燥物料的出料口，出料口连接真空出料机构。
更优选地，所述真空喷雾冷冻造粒装置的喷雾筒与动态加热干燥装置的外筒连接组成完整的密闭容器。
更优选地，所述真空出料机构用于将干燥物料从真空密闭容器中放出，恢复到大气压下分装至收料罐或连接到其他收料装置，所述机构由上出料阀、缓存区、复压管道、抽气管道及下出料阀组成。
进一步地，上出料阀、下出料阀设于所述动态加热干燥装置出料口下方，上出料阀、下出料阀之间设有缓存区，缓存区通过设有抽气阀的管路与所述动态加热干燥装置的外筒连接，缓存区还连接设有复压阀的干燥洁净无菌气体通入管路；收料装置与下出料阀连接。
优选地，所述回转干燥器包括
用于容纳并加热干燥物料的转筒；
用于将转筒与电机连接的转轴；
用于给转轴旋转提供动力的电机。
优选地，所述转筒的全部、转轴的一部分设于密闭容器内，所述转轴的另一部分在密闭容器外部与所述电机连接。
进一步地，所述转轴与外筒之间通过轴座连接。
优选地，所述转筒外侧设有至少一段中空夹套，中空夹套内通流体使筒壁升温或降温。
进一步地，所述中空夹套截面形状为矩形，以环绕所述转筒外部一周的形式设置；中空夹套为一段或多段，沿其旋转中心线方向直线排列；每段中空夹套均设有流体进、出管道，内部通流体循环使筒壁升温或降温。
优选地，所述转筒内壁设有至少一段与转筒旋转中心线呈一定角度的导向槽，当转筒正向旋转，物料被导向槽带动向出料口方向迁移；当转筒反向旋转，物料被带回。
优选地，所述控温循环系统包括依次连接组成一个闭合回路的旋转接头、热交换器、电加热器及流体泵，闭合回路内通循环流体。
更优选地，所述旋转接头是一侧用于固定连接，一侧用于连接回转体并在回转体任意旋向连续或不连续旋转运动中不间断地输送流体，不间断地输送电流的装置。
进一步地，所述转轴内部设有用于流体循环的通道，该通道一侧在所述外筒容器内与所述转筒上的一段或多段中空夹套连接；该通道另一侧在所述外筒容器外与所述旋转接头连接。旋转接头在转轴任意旋向连续或不连续旋转运动中，使所述闭合回路内的流体在所述中空夹套内不间断地输送。
进一步地，所述流体为水或硅油。
进一步地，所述转筒内设有用于检测物料信息的探测器，所述信息可以是温度；探测器与所述旋转接头连接；所述旋转接头在转轴任意旋向连续或不连续旋转运动中不间断地输送电流。
优选地，所述全自动密闭式喷雾冻干生产设备还包括将洁净水引入密闭容器内进行清洗，及将消毒剂引入密闭容器内进行灭菌的清洗灭菌系统，所述消毒剂可以是无菌纯蒸汽。
优选地，所述的全自动密闭式喷雾冻干生产设备还包括用于对真空喷雾冷冻造粒及动态加热干燥过程进行程序自动控制的控制系统，所述的控制系统包括可编程逻辑控制器(PLC)和计算机(PC)中的至少一个。
本发明还提供了一种全自动密闭式喷雾冻干生产方法，采用上述的全自动密闭式喷雾冻干生产设备，步骤为：
步骤1：选择性打开或关闭所述设备的各个阀门，利用真空系统将密闭容器抽到一定的真空度；
步骤2：利用雾化喷嘴将待冻干液体雾化分散为液滴并喷入喷雾筒，所述的液滴中的部分组分在真空环境中汽化吸热使液滴温度下降，所述的冷凝装置将汽化后的所述的液滴中的部分组分凝结进而维持所述的容器中的真空度，液滴温度持续下降直至冻结形成冰颗粒；
步骤3：通过进料管将所述冰颗粒物料加入转筒中；转筒温度通过控温循环系统控制；转筒在干燥过程中持续转动，物料在转筒底部翻滚，充分均匀地与筒壁接触受热；导向槽随转筒旋转将物料从转筒底部带起，物料由于重力作用在导向槽上向出料口方向滑动，当导向槽随转筒继续旋转，物料由于重力作用跌落回转筒底部；通过控制喷雾加料量与转筒转速使物料以适当的速率向出料口迁移并均匀散布在转筒底部，不形成堆积，升华气体快速从物料表面及颗粒间隙中排出通过真空系统抽走并凝结在冷凝装置表面；物料通过转筒转动持续翻滚和逐步向前迁移的复合运动，在转筒内逐渐干燥，直至完全干燥；
步骤4：干燥物料从转筒内掉落到出料口内；需要出料时，打开上出料阀，物料落入缓存区，关闭上出料阀、抽气阀；打开复压阀，向缓存区通入干燥洁净无菌气体，使缓存区与收料装置内外压差一致；打开下出料阀，通过收料装置收集干燥物料，缓存区物料排净后关闭下出料阀、复压阀，打开抽气阀，并且更换收料装置；需要再次出料时，重复该步骤。
与现有技术相比，本发明具有如下有益效果：
1、通过真空喷雾冷冻造粒技术将液体冻结成颗粒，极大地提高了待冻干液体的冷冻速率，喷雾筒内不设置冷媒喷嘴，装置内不具有液氮低温区，速冻过程中完全不使用冷媒与物料接触，完全杜绝物料被污染的风险，提高了冻干工艺的无菌性，降低了生产能耗，并且冷媒是循环使用的，不向环境排放产生污染。
2、通过回转干燥器使冻干物料在转筒内动态翻滚，充分、均匀受热，并使升华气体快速排出，提高了干燥效率，缩短了物料的干燥时间；物料在加热干燥装置中主要依靠自身重力进行翻滚或迁移，其原有的形体状态得以保护；并且使干燥过程可以连续进行。
3、通过真空出料机构将冻干后物料从真空密闭环境内转移到常压下，保证冻干工艺可以连续进行，保护密闭容器不受环境污染。
4、整个冻干生产中设备保持系统密闭，从待冻干液体加入到干燥颗粒放出， 所有加料、冷冻干燥、出料过程均在无菌密闭的环境中进行，降低了物料被环境污染或污染环境的风险；且整个过程可以连续进行，保证了冻干工艺的密闭性、无菌性和连续性。
5、相较于传统冻干工艺生产流程简化，生产效率提高，自动化程度提高，能耗降低，设备运行和维护成本降低；
6、适用范围较广，大部分的注射剂和无菌原料药均可采用该设备进行冻干，包括很多不适合使用传统冻干机冻干的蛋白类制剂、生物制品及有毒、致敏性物料等。
附图说明
图1为传统的冷冻干燥装置的结构示意图；
图2为实施例1提供的全自动密闭式喷雾冻干生产设备的结构示意图；
图3为实施例1中真空喷雾冷冻造粒装置的结构示意图；
图4为实施例1中动态加热干燥装置的结构示意图；
图5为实施例1中真空出料机构的结构示意图；
图6为实施例2提供的全自动密闭式喷雾冻干生产设备的结构示意图；
图7为实施例2中真空喷雾冷冻造粒装置的结构示意图；
图8为实施例3提供的全自动密闭式喷雾冻干生产设备的结构示意图；
图9为实施例3中真空喷雾冷冻造粒装置的结构示意图；
图10为实施例4中动态加热干燥装置的结构示意图。
具体实施方式
下面结合具体实施例，进一步阐述本发明。应理解，这些实施例仅用于说明本发明而不用于限制本发明的范围。此外应理解，在阅读了本发明讲授的内容之后，本领域技术人员可以对本发明作各种改动或修改，这些等价形式同样落于本申请所附权利要求书所限定的范围。
实施例1
图2为本实施例提供的全自动密闭式喷雾冻干生产设备的结构示意图，所述的设备包括依次连接形成密闭容器的真空喷雾冷冻造粒装置1、动态加热干燥装 置2及真空出料机构3。
图3为本实施例提供的真空喷雾冷冻造粒装置1的结构示意图，所述的装置包括用于在喷雾造粒过程中容纳产品的喷雾筒1-1；多个用于将待冻干液体雾化分散为液滴并喷入喷雾筒1-1中的雾化喷嘴1-2；用于在密闭容器中形成真空环境使所述的液滴中的部分组分在该真空环境中汽化吸热进而使液滴降温冻结形成冰颗粒的真空系统；以及用于将汽化后的所述的液滴中的部分组分冷凝的冷凝装置。所述的雾化喷嘴1-2设于喷雾筒1-1内。所述的真空系统与喷雾筒1-1连接。
所述的喷雾筒1-1上部为筒形，下部为锥形。所述的冷凝装置为设于喷雾筒1-1上部的外侧通入冷媒的第一制冷夹套1-3，冷媒为硅油。硅油通过管道上的流体泵1-4形成循环并通过热交换器1-5降温。第一制冷夹套1-3的截面为矩形，以环绕喷雾筒1-1的上部一圈的形式设置。喷雾筒1-1的下部锥形外侧设有用于避免冰颗粒融化的第二制冷夹套1-6，其内通入冷媒为硅油。硅油通过另一组管道上的流体泵1-4形成循环并通过热交换器1-5降温。第二制冷夹套1-6的截面为矩形，以环绕喷雾筒1-1下部锥形外侧一圈的形式设置。所述的两个热交换器1-5都连接制冷系统1-7。所述的制冷系统1-7为压缩机。
所述的雾化喷嘴1-2连接密闭的配液管道1-8，管道内通入待冻干液体，配液管道1-8上设有流量调节阀1-9。所述的真空系统包括真空泵1-10，与喷雾筒1-1通过管道1-11连接，所述的管道1-11上设有阀门1-12。喷雾筒1-1的连接口上设有过滤网1-13。
所述的喷雾筒1-1的底部设有用于放出冰颗粒的出料阀1-14，喷雾筒1-1的顶壁、上部侧壁和下部侧壁的外侧各设有一个用于把冰颗粒震落的振动器1-15。所述的振动器1-15由电机驱动振动。所述的出料阀1-14通过管道与动态加热干燥装置连接。
图4为本实施例提供的动态加热干燥装置2的结构示意图，所述的装置包括：外筒2-1、进料管2-2、出料口2-4，出料口有阀门；所述喷雾筒1-1通过出料阀1-14与进料管2-2连接，喷雾筒1-1与外筒2-1组成密闭容器并保护容器内物料不受环境污染或污染环境；由转筒2-11、转轴2-12、电机2-13，以及至少一个轴座组成的回转干燥器，转筒2-11用于容纳并加热干燥物料，转轴2-12用于将 电机2-13旋转动力传递给转筒2-11；由旋转接头2-21、热交换器2-22、电加热器2-23、流体泵2-24组成的控温循环系统。
转筒2-11外侧设有至少一段中空夹套2-15，每段中空夹套2-15均通过管道与转轴2-12内部的通道连接，并且转筒2-11的全部、转轴2-12的一部分安装在密闭容器内；转轴2-12的另一部分在密闭容器外与电机2-13连接，并且该部分的内部通道与旋转接头2-21连接；所述的旋转接头2-21是一侧用于固定连接，另一侧用于连接转轴2-12并在其任意旋向连续或不连续旋转运动中不间断地输送流体，不间断地输送电流的装置。所述的控温循环系统内通入流体为硅油，硅油通过电加热器2-23加热并通过热交换器2-22调节温度并通过流体泵2-24进行循环流动使中空夹套2-15筒壁升温或降温。
图5为本实施例提供的真空出料机构3的结构示意图，所述的机构包括设于出料口2-4下方的上出料阀3-1、下出料阀3-2，及两出料阀之间的缓存区3-3，缓存区3-3通过带有抽气阀3-5的管路与密闭容器连接，缓存区3-3还连接带有复压阀3-6的通入干燥洁净无菌气体的管路；收料罐3-4与下出料阀3-2连接。
所述的设备的密闭容器内还可通入洁净水用于容器清洗，可通入消毒剂用于容器灭菌，消毒剂优选无菌蒸汽。
上述全自动密闭式喷雾冻干生产设备使用时，待冻干液体可以是常温水溶液、混悬液、乳浊液等，包含或不包含辅料均可，以将125g常青藤粉末溶解于2L水中所得的常青藤粉末水溶液为例，包括如下步骤：
步骤1：先利用真空系统将所述的喷雾筒1-1与外筒2-1组成的密闭容器抽到负压，真空度为300Pa。
步骤2：所述的第一制冷夹套1-3温度控制为-60℃，第二制冷夹套1-6温度控制为-20℃；通过配液管道1-8将所述的常青藤粉末水溶液输送给雾化喷嘴1-2，喷雾压力为0.4MPa，喷嘴直径为1.0mm，利用雾化喷嘴1-2将液体雾化分散为液滴并喷入喷雾筒1-1，液滴中的水在真空环境中汽化后吸热使液滴温度下降，真空系统持续抽真空，所述的第一制冷夹套1-3将汽化后的水凝结在喷雾筒1-1内壁进而维持真空度，液滴温度持续下降直至冻结形成冰颗粒，该过程仅需数秒完成，通过振动器1-15的振动作用将冰颗粒震落到喷雾筒1-1底部放出。所述的液滴在喷雾筒1-1内不与冷媒直接接触而被冻结。
步骤3：通过进料管2-2将物料的冰颗粒加入到转筒2-11内。所述的转筒2-11某一段中空夹套2-15通过控温循环系统控制加热温度为20℃；转筒2-11在干燥过程中持续旋转，物料在转筒底部翻滚，充分均匀地与筒壁接触受热；导向槽2-14随转筒旋转将物料从转筒底部带起，物料由重力作用在导向槽上向出料口2-4方向滑动，导向槽随转筒继续旋转，物料由重力作用跌落回转筒底部，通过控制流量调节阀1-9的液体加入量与转筒转速使物料以适当的速率向出料口迁移并均匀散布在转筒底部，不形成堆积；升华气体快速从物料表面及颗粒间隙中排出通过真空系统抽走并凝结在喷雾筒1-1上部内壁；物料通过转筒旋转持续翻滚和逐步向出料口迁移的复合运动，在转筒内逐渐干燥，直至完全干燥。
步骤4：干燥物料从转筒2-11内掉落到出料口2-4内；需要出料时，打开上出料阀3-1，物料落入缓存区3-3内，关闭上出料阀3-1、抽气阀3-5；打开复压阀3-6，向缓存区通入干燥洁净无菌气体，使缓存区3-3与收料装置3-4内外压差一致；打开下出料阀3-2，通过收料装置3-4收集干燥物料，缓存区3-3内物料排净后关闭下出料阀、复压阀，打开抽气阀，并且更换收料装置；需要再次出料时，重复该步骤。
所述的全自动密闭式喷雾冻干生产设备在冻干过程中通过由可编程逻辑控制器和计算机组成的控制系统进行自动化控制。
实施例2
图6为实施例2提供的全自动密闭式喷雾冻干生产设备的结构示意图，该实施例与实施例1的区别在于真空喷雾冷冻造粒装置部分。
如图7所示，为实施例2中的真空喷雾冷冻造粒装置结构示意图，所述装置类似于实施例1，区别在于：所述的冷凝装置为设于喷雾筒1-1外并与其连接的冷凝器1-30，所述的冷凝器1-30通过管道1-11连接喷雾筒1-1的连接口，所述的真空泵1-10通过另一管道连接冷凝器1-30，冷凝器1-30与喷雾筒1-1的连接管道1-11上设有阀门1-12，喷雾筒1-1上部的外侧不设置第一制冷夹套1-3。
以将125g常青藤粉末溶解于2L水中所得的常青藤粉末水溶液为例，上述全自动密闭式喷雾冻干生产设备使用时，实施步骤类似于实施例1，区别在于：
步骤2：所述液体速冻过程中液滴喷入喷雾筒1-1，水在真空环境中汽化后吸热使液滴温度下降，真空系统持续抽真空，所述的冷凝器1-30将汽化后的水 凝结进而维持容器内真空度，液滴温度持续下降直至冻结形成冰颗粒。
步骤3：所述冰颗粒物料在加热干燥过程中升华气体排出，通过真空系统抽走并凝结在所述冷凝器1-30上。
实施例3
图8为实施例3提供的全自动密闭式喷雾冻干生产设备的结构示意图，该实施例与实施例1的区别在于真空喷雾冷冻造粒装置部分。
如图9所示，为实施例3中的真空喷雾冷冻造粒装置结构示意图，所述装置类似于实施例1，区别在于：所述的冷凝装置为第一制冷夹套1-3与冷凝器1-30的组合，所述的第一制冷夹套1-3设于喷雾筒1-1上部的外侧，所述的冷凝器1-30设于喷雾筒1-1外；所述的冷凝器1-30通过管道1-11连接喷雾筒1-1的连接口，所述的真空泵1-10通过另一管道连接冷凝器1-30，冷凝器1-30与喷雾筒1-1的连接管道1-11上设有阀门1-12。
以将125g常青藤粉末溶解于2L水中所得的常青藤粉末水溶液为例，上述全自动密闭式喷雾冻干生产设备使用时，实施步骤类似于实施例1，区别在于：
步骤2：所述液体速冻过程中液滴喷入喷雾筒1-1，水在真空环境中汽化后吸热使液滴温度下降，真空系统持续抽真空，所述的第一制冷夹套1-3将汽化后的水凝结在喷雾筒1-1内壁，冷凝器1-30将汽化后的水凝结，进而维持容器内真空度，液滴温度持续下降直至冻结形成颗粒。
步骤3：所述冰颗粒物料在加热干燥过程中升华气体排出，通过真空系统抽走并凝结在所述喷雾筒1-1上部内壁和冷凝器1-30上。
本实施例提供的所述真空喷雾冷冻造粒装置的喷雾筒1-1外部连接多个冷凝器1-30，所述设备连续的进行喷雾冻干生产。
实施例4
图2为实施例4提供的全自动密闭式喷雾冻干生产设备的结构示意图，结合图5、图10，本实施例的结构可以与实施例1、2、3相同，实施步骤不同。
以将125g常青藤粉末溶解于2L水中所得的常青藤粉末水溶液为例，上述全自动密闭式喷雾冻干生产设备使用时，实施步骤的区别在于：
步骤2：所述液体速冻过程中液滴喷入喷雾筒1-1，冻结形成一定批量的冰颗粒后停止喷雾。
步骤3：通过进料管2-2将冻结成冰颗粒的物料加入转筒2-11内。加料过程中转筒2-11旋转，物料在转筒底部翻滚，此时控温循环系统不加热中空夹套2-15；加料完毕，控温循环系统开始加热，转筒2-11通过电机2-13驱动正转一段时间后反转，经过若干次旋转方向切换，物料在转筒内左右迁移逐渐干燥；直至该次加入的物料完全干燥。
步骤4：需要出料时，依次打开真空出料机构的复压阀3-6、抽气阀3-5，向缓存区3-3和密闭容器内通入干燥洁净无菌气体，使容器的压力与收料装置3-4压差一致，打开上出料阀3-1、下出料阀3-2，使出料口2-4与收料装置3-4接通，转筒2-11连续正转直至物料排空。
本实施例使用全自动密闭式喷雾冻干生产设备批次的冻干生产物料。

Claims (10)

  1. 一种全自动密闭式喷雾冻干生产设备，其特征在于：包括互相连接组成密闭容器的真空喷雾冷冻造粒装置(1)和动态加热干燥装置(2)；
    真空喷雾冷冻造粒装置(1)包括喷雾筒(1-1)，所述喷雾筒(1-1)内设有用于将待冻干液体雾化分散为液滴的雾化喷嘴(1-2)，所述喷雾筒(1-1)连接用于在密闭容器中形成真空环境使所述的液滴中的部分组分在该真空环境中汽化吸热进而使液滴降温冻结形成冰颗粒的真空系统；
    动态加热干燥装置(2)包括外筒(2-1)；用于容纳并加热物料的回转干燥器部分设于外筒(2-1)内；用于控制回转干燥器加热温度的控温循环系统与回转干燥器连接。
  2. 如权利要求1所述的全自动密闭式喷雾冻干生产设备，其特征在于：所述真空喷雾冷冻造粒装置(1)还包括用于将汽化后的所述的液滴中的部分组分冷凝的冷凝装置；
    所述冷凝装置为第一制冷夹套(1-3)和冷凝器(1-30)中的一种或其组合，所述的第一制冷夹套(1-3)设于所述喷雾筒(1-1)上部的外侧，第一制冷夹套(1-3)内部通有冷媒；所述冷凝器(1-30)设于所述喷雾筒(1-1)外，并与所述喷雾筒(1-1)连接。
  3. 如权利要求2所述的全自动密闭式喷雾冻干生产设备，其特征在于：所述的真空系统包括真空泵(1-10)，所述喷雾筒(1-1)设有连接口，所述连接口上设有阀门；当所述的冷凝装置为第一制冷夹套(1-3)时，所述的真空泵(1-10)通过管道(1-11)连接所述的喷雾筒(1-1)的连接口；当所述的冷凝装置为冷凝器(1-30)或第一制冷夹套(1-3)和冷凝器(1-30)的组合时，所述的冷凝器(1-30)通过管道(1-11)连接所述的喷雾筒(1-1)的连接口，所述的真空泵(1-10)通过另一管道连接冷凝器(1-30)。
  4. 如权利要求3所述的全自动密闭式喷雾冻干生产设备，其特征在于：所述液滴中的部分组分为水；
    所述液滴在所述密闭容器内不与冷媒接触；
    所述喷雾筒(1-1)为所述密闭容器的一部分；所述喷雾筒(1-1)上部为筒形，下部为锥形；
    所述的喷雾筒(1-1)的下部的外侧设有用于避免冰颗粒融化的第二制冷夹套(1-6)，所述的第二制冷夹套(1-6)内通有冷媒；
    所述的喷雾筒(1-1)的底部设有用于放出冰颗粒的下料管(1-14)；
    所述雾化喷嘴(1-2)连接密闭的配液管道(1-8)，所述配液管道(1-8)上设有流量调节装置(1-9)。
  5. 如权利要求4所述的全自动密闭式喷雾冻干生产设备，其特征在于：所述外筒(2-1)为所述密闭容器的一部分，所述外筒(2-1)上设有
    用于连接所述真空喷雾冷冻造粒装置(1)的所述下料管(1-14)的进料管(2-2)；
    及用于放出干燥物料的出料口(2-4)。
  6. 如权利要求1所述的全自动密闭式喷雾冻干生产设备，其特征在于：所述回转干燥器包括
    用于容纳并加热干燥物料的转筒(2-11)；
    用于将转筒(2-11)与电机(2-13)连接的转轴(2-12)；
    用于给所述转轴(2-12)旋转提供动力的电机(2-13)。
  7. 如权利要求6所述的全自动密闭式喷雾冻干生产设备，其特征在于：所述转筒(2-11)的全部、转轴(2-12)的一部分设于密闭容器内，所述转轴(2-12)的另一部分在密闭容器外与所述电机(2-13)连接，所述转轴(2-12)与外筒(2-1)之间通过轴座连接；
    所述转筒(2-11)外侧设有至少一段中空夹套(2-15)，中空夹套(2-15)内通流体使筒壁升温或降温；
    所述转筒(2-11)内壁设有至少一段与转筒旋转中心线呈一定角度的导向槽(2-14)，当转筒(2-11)正向旋转，物料被导向槽(2-14)带动向出料口方向迁移；当转筒(2-11)反向旋转，物料被带回。
  8. 如权利要求7所述的全自动密闭式喷雾冻干生产设备，其特征在于：所述控温循环系统包括依次连接组成一个闭合回路的旋转接头(2-21)、热交换器(2-22)、电加热器(2-23)及流体泵(2-24)，闭合回路内通循环流体；
    所述转轴(2-12)内部设有用于流体循环的通道，该通道一侧在所述密闭容器内与所述转筒(2-11)上的一段或多段中空夹套(2-15)连接；该通道另一侧 在密闭容器外与所述旋转接头(2-21)连接；所述旋转接头(2-21)在转轴(2-12)任意旋向连续或不连续旋转运动中，使所述闭合回路内的流体在所述中空夹套(2-15)内不间断地输送；
    所述转筒(2-11)内设有用于检测物料信息的探测器，所述探测器与所述旋转接头(2-21)连接，所述旋转接头(2-21)在转轴(2-12)任意旋向连续或不连续旋转运动中不间断地输送电流。
  9. 如权利要求8所述的全自动密闭式喷雾冻干生产设备，其特征在于：还包括用于将干燥物料从真空密闭容器内放出，恢复到大气压下分装并收料的真空出料机构(3)；
    所述真空出料机构(3)包括设于所述动态加热干燥装置(2)出料口(2-4)下方的上出料阀(3-1)、下出料阀(3-2)，上出料阀(3-1)、下出料阀(3-2)之间设有缓存区(3-3)，缓存区(3-3)通过设有抽气阀(3-5)的管路与所述动态加热干燥装置(2)的外筒连接，缓存区(3-3)还连接设有复压阀(3-6)的干燥洁净无菌气体通入管路；收料装置(3-4)与下出料阀(3-2)连接。
  10. 一种全自动密闭式喷雾冻干生产方法，其特征在于，采用如权利要求9所述的全自动密闭式喷雾冻干生产设备，步骤为：
    步骤1：选择性打开或关闭所述设备的各个阀门，利用真空系统将真空喷雾冷冻造粒装置(1)和动态加热干燥装置(2)互相连接组成的密闭容器抽到一定的真空度；
    步骤2：利用雾化喷嘴(1-2)将待冻干液体雾化分散为液滴并喷入喷雾筒(1-1)，所述的液滴中的部分组分在真空环境中汽化吸热使液滴温度下降，所述的冷凝装置将汽化后的所述的液滴中的部分组分凝结进而维持所述的密闭容器中的真空度，液滴温度持续下降直至冻结形成颗粒；
    步骤3：通过进料管(2-2)将所述冰颗粒物料加入转筒(2-11)中；转筒(2-11)温度通过控温循环系统控制；转筒(2-11)在干燥过程中持续转动，物料在转筒(2-11)底部翻滚，充分均匀地与筒壁接触受热；导向槽(2-14)随转筒(2-11)旋转将物料从转筒(2-11)底部带起，物料由于重力作用在导向槽(2-14)上向出料口(2-4)方向滑动，当导向槽(2-14)随转筒继续旋转，物料由于重力作用跌落回转筒(2-11)底部；通过控制喷雾加料量与转筒(2-11)转速使物料以 适当的速率向出料口(2-4)迁移并均匀散布在转筒底部，不形成堆积，升华气体快速从物料表面及颗粒间隙中排出通过真空系统抽走并凝结在冷凝装置表面，物料通过转筒(2-11)转动持续翻滚和逐步向前迁移的复合运动，在转筒(2-11)内逐渐干燥，直至完全干燥；
    步骤4：干燥物料从转筒(2-11)内掉落到出料口(2-4)内；需要出料时，打开上出料阀(3-1)，物料落入缓存区(3-3)，关闭上出料阀(3-1)、抽气阀(3-5)；打开复压阀(3-6)，向缓存区通入干燥洁净无菌气体，使缓存区(3-3)与收料装置(3-4)内外压差一致；打开下出料阀(3-2)，通过收料装置(3-4)收集干燥物料，缓存区(3-3)物料排净后关闭下出料阀(3-2)、复压阀(3-6)，打开抽气阀(3-5)，并且更换收料装置(3-4)；需要再次出料时，重复步骤4。
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