CN105318665A - Full-automatic closed spray freeze-drying production equipment and method - Google Patents
Full-automatic closed spray freeze-drying production equipment and method Download PDFInfo
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- CN105318665A CN105318665A CN201510790555.5A CN201510790555A CN105318665A CN 105318665 A CN105318665 A CN 105318665A CN 201510790555 A CN201510790555 A CN 201510790555A CN 105318665 A CN105318665 A CN 105318665A
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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
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- 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
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Abstract
The invention provides full-automatic closed spray freeze-drying production equipment. The production equipment comprises a vacuum spray-freezing pelletizing device, a dynamic heating drying device and a vacuum discharging mechanism, wherein the vacuum spray-freezing pelletizing device comprises a spray barrel, atomizing nozzles used for atomizing and dispersing liquid to be freeze-dried into liquid drops are arranged in the spray barrel, and the spray barrel is connected with a vacuum system which forms a vacuum environment in a container to enable part of components in the liquid drops to be vaporized in the vacuum environment so as to absorb heat, and then the liquid drops are frozen to form particles; the dynamic heating drying device comprises an outer barrel used for forming the closed container, a rotary drier used for containing and heating dry materials is partially arranged in the closed container, and a heating circulation system controls the temperature of the rotary drier; the vacuum discharging mechanism is used for discharging the dry materials from the vacuum closed container. The invention further provides a full-automatic closed spray freeze-drying production method. Freeze-drying is carried out under the closed condition, and no refrigerants are adopted to make contact with the materials, so that the risk of medicine pollution is lowered; the process can be continuous, and airtightness, sterility and continuity of spray freeze-drying production are guaranteed.
Description
Technical field
The present invention relates to a kind of full-automatic enclosed formula spraying freeze-drying production equipment, for aseptic freeze-dried workshop, pharmaceutical factory, belong to Vacuum Freezing & Drying Technology field.
Background technology
Vacuum freeze drying, also claims lyophilization.Its principle be in closed environment by treating that the solution of freeze-drying carries out freezing, then give certain temperature and vacuum, make the moisture in frozen solution by distillation mode remove.
Vacuum freeze drying has following advantage:
(1) under low temperature, freeze-drying medicine can not cause medicine sex change or loss of activity occurs.
(2) in the medicine of freeze-drying, the catalytic action of microbial growth and enzyme almost can not occur.
(3) by freeze-drying, medicine can the initial volume of extraordinary maintenance and shape.
(4) easily oxidized in medicine composition can be protected easily.
(5) long-term preservation is beneficial to.
(6) most of freeze-drying medicine can at room temperature store.
Based on above-mentioned advantage, Freeze Drying Technique may be used for following field: the production of food and microorganism, the production of the medicine being representative with injection bulk drug, the production and processing of blood product, and the manufacture of other material various and processing.
In traditional freeze drying process, as shown in Figure 1, need to treat that the liquid A of freeze-drying is filled in the container B such as vial or pallet in advance, again this container B is contained in plane place flaggy C on glaciation, under vacuum environment, flaggy heats up to ice cube heating, and steam sublimation also leaves dry matter.In this dry run, material to be dried is standing all the time, only have bottom among a small circle region contact with flaggy, conduct heat limited, particularly when material load in advance carry out freeze-drying in the container of the hot non-conductors such as vial time, heat-transfer effect is poor, and drying time is long; The material upper surface left standstill is dry at first, and drying layer declines to frozen crust gradually, and at this one-phase, drying layer becomes the obstruction of frozen crust distillation steam to external diffusion, and mass transfer effect is poor, extends drying time further; In addition, standing and drying it is also proposed very high requirement to flaggy temperature homogeneity.
Publication number be US20130118026A1 U.S. patents disclose a kind of spray freeze-drying technique, its be by treat freeze-drying liquid from container side's nozzle spray under, another group nozzle sprays liquid nitrogen, treat in freeze-drying droplets fall process with refrigerant contact heat-exchanging, quick-frozen forms ice particle; Ice particle is placed in conical vessel, uses agitator to stir, by cone wall heat drying material; Agitator stirs and applies mechanical force to material, and its friction, collision effect easily destroy the original body state of material; And material must be stacked into certain altitude and can be stirred by agitator in cone, this accumulation also hinders bottom distillation steam to external diffusion; In addition, cone drier gradation can only carry out drying.
Separately have a kind of Technique of Speed Freezing to be that liquid nitrogen is placed in container bottom, treat freeze-drying liquid from top spray or drip, carry out quick-frozen through liquid nitrogen cryogenics district.In pharmaceuticals industry that freeze drying process is widely used in (but being not limited to), its goods have strict demand to cleaning, aseptic pharmaceutical technology.Above two kinds of Techniques of Speed Freezing all use refrigerant (liquid nitrogen) directly to contact refrigeration with material, its cleanliness factor, aseptic are difficult to ensure, and vaporize after refrigerant heat exchange, again make liquid state and need consume very big energy, directly discharge then easily causes waste and pollutes.
In sum, how to improve in freeze drying process and treat the freezing of freeze-dried material and drying efficiency, and this process should be avoided destroying the original body state of material as far as possible; The more important thing is in freeze-dry process, how to protect material cleanliness factor and aseptic, avoid material to carry by environmental pollution or contaminated environment between devices; Further make freeze drying carry out continuously, reduce energy consumption simultaneously, all become those skilled in the art's problem demanding prompt solution.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of can raising in freeze drying process and treats the freezing of freeze-drying liquid and drying efficiency; keep the freezing rear original body state of material simultaneously; the cleanliness factor of protection goods and aseptic; the spraying freeze-drying production equipment that freeze drying is carried out continuously, to shorten lyophilization cycle, enhance productivity, reduce the contaminated risk of medicine, to reduce costs and energy consumption.
For solving the problems of the technologies described above, technical scheme of the present invention is to provide a kind of full-automatic enclosed formula spraying freeze-drying production equipment, it is characterized in that: comprise the freezing prilling granulator of vacuum spraying and dynamic heat drying device that are connected to each other composition closed container;
The freezing prilling granulator of described vacuum spraying comprises cannon spray head, be provided with for treating that the freeze-drying atomization of liquid is separated into the atomizer of drop in described cannon spray head, described cannon spray head connects and is used for being formed vacuum environment in closed container the constituent part in described drop vaporize heat absorption and then drop is lowered the temperature freeze the vacuum system of formation ice particle in this vacuum environment.
Preferably, the constituent part in described drop is water.
Preferably, described drop does not directly contact with refrigerant in closed container.
Preferably, described cannon spray head is a part for closed container, and top is tubular, and bottom is taper.
Preferably, described atomizer connects airtight dosing pipeline, and described dosing pipeline is provided with flow regulator.
Preferably, the freezing prilling granulator of described vacuum spraying also comprises for the condensing unit by the constituent part condensation in the described drop after vaporization.
More preferably, described condensing unit is one in the first refrigeration chuck and condenser or its combination, and the first described refrigeration chuck is located at the outside on described cannon spray head top, and the first refrigeration chuck inside is connected with refrigerant; Described condenser is located at outside described cannon spray head, and is connected with described cannon spray head.
Preferably, described vacuum system comprises vavuum pump, and described cannon spray head is provided with connector, and connector is provided with valve; When described condensing unit is the first refrigeration chuck, vavuum pump connects the connector of cannon spray head by pipeline; When described condensing unit is the combination of condenser or the first refrigeration chuck and condenser, condenser connects the connector of cannon spray head by pipeline, and vavuum pump connects condenser by another pipeline.
Further, the connector of described cannon spray head is provided with screen pack.
Further, the refrigerant in described first refrigeration chuck is formed circulation by the fluid pump on pipeline and is lowered the temperature by heat exchanger.
Further, the cross section of described first refrigeration chuck is rectangle, arranges with the form of enclosing around the top one of described cannon spray head; Or the cross section of described first refrigeration chuck is semicircle, and the form spirally around the some circles in top of described cannon spray head is arranged, the refrigerant in the first described refrigeration chuck can be silicone oil.
Further, described refrigerant temperature is-40 DEG C ~-100 DEG C.
Preferably, being provided with the second refrigeration chuck for avoiding ice particle to melt outside the lower taper of described cannon spray head, in the second refrigeration chuck, being connected with refrigerant.
Further, the refrigerant in described second refrigeration chuck is formed circulation by the fluid pump on pipeline and is lowered the temperature by heat exchanger.
Further, the cross section of described second refrigeration chuck is rectangle, arranges with the form of enclosing around tapered outer side one; Or the cross section of the second described refrigeration chuck is semicircle, and the form spirally around the some circles of tapered outer side is arranged, the refrigerant in the second described refrigeration chuck can be silicone oil.
Further, the refrigerant temperature in the second described refrigeration chuck is-10 DEG C ~-40 DEG C.
Preferably, the tremie pipe for releasing ice particle is provided with bottom described cannon spray head.
More preferably, the outside of the roof of described cannon spray head, upper portion side wall and tapered sidewalls is provided with at least one for ice particle being shaken off the vibrator in tremie pipe.
More preferably, described tremie pipe is connected with described dynamic heat drying device, and the pipeline be connected has valve.
Described dynamic heat drying device comprises urceolus; Rotary dryer part for holding also heated material is located in urceolus; Temperature controlling circulating system for controlling rotary dryer heating-up temperature is connected with rotary dryer.
Preferably, described urceolus is a part for closed container, and urceolus is provided with
For connecting the feed pipe of the freezing prilling granulator tremie pipe of vacuum spraying;
And for releasing the discharging opening of dried material, discharging opening connects Vacuum discharge mechanism.
More preferably, the cannon spray head of the freezing prilling granulator of described vacuum spraying and the urceolus of dynamic heat drying device connect to form complete closed container.
More preferably, described Vacuum discharge mechanism is used for dried material to release from vacuum airtight container, return to lower point of atmospheric pressure be filled to rewinding tank or be connected to other material collecting devices, described mechanism is made up of top discharge valve, buffer area, multiple pressure pipeline, pump-line and bottom discharge valve.
Further, top discharge valve, bottom discharge valve are located at below described dynamic heat drying device discharging opening, buffer area is provided with between top discharge valve, bottom discharge valve, buffer area is connected with the urceolus of described dynamic heat drying device by the pipeline being provided with extraction valve, and the dried and clean aseptic gas that buffer area is also connected with multiple pressure valve passes into pipeline; Material collecting device is connected with bottom discharge valve.
Preferably, described rotary dryer comprises
For holding and the rotating cylinder of heat drying material;
For the rotating shaft that rotating cylinder is connected with motor;
For giving the motor of rotating shaft powered rotation.
Preferably, a part that is whole, rotating shaft for described rotating cylinder is located in closed container, and another part of described rotating shaft is connected with described motor in closed container outside.
Further, described rotating shaft is connected by axle bed with between urceolus.
Preferably, be provided with at least one section of hollow jacket outside described rotating cylinder, in hollow jacket, through-flow body makes barrel heat up or cooling.
Further, described hollow jacket cross sectional shape is rectangle, to arrange around the described rotating cylinder form of outside a week; Hollow jacket is one or more snippets, arranged in a straight line along its rotation centerline direction; Every section of hollow jacket is equipped with fluid into and out of pipeline, and inner through-flow body circulation makes barrel heat up or cooling.
Preferably, described rotating cylinder inwall be provided with at least one section with rotating cylinder rotation centerline gathering sill at an angle, when rotating cylinder rotates forward, material be directed to groove band trend discharging opening direction migration; When rotating cylinder reversely rotates, material is brought back.
Preferably, described temperature controlling circulating system comprises the swivel joint, heat exchanger, electric heater and the fluid pump that connect to form a closed-loop path successively, logical circulation of fluid in closed-loop path.
More preferably, described swivel joint be side for being fixedly connected with, the device of electric current, for connecting revolving body and carrying fluid in any rotation direction of revolving body incessantly in continuous or discontinuous rotary motion, is carried incessantly in side.
Further, described rotating shaft inside is provided with the passage for fluid circulation, and this passage side is connected with one or more snippets hollow jacket on described rotating cylinder in described urceolus container; This passage opposite side is connected with described swivel joint outside described urceolus container.Swivel joint in continuous or discontinuous rotary motion, makes the fluid in described closed-loop path carry incessantly in described hollow jacket in any rotation direction of rotating shaft.
Further, described fluid is water or silicone oil.
Further, be provided with the detector for detecting material information in described rotating cylinder, described information can be temperature; Detector is connected with described swivel joint; Described swivel joint carries electric current in any rotation direction of rotating shaft in continuous or discontinuous rotary motion incessantly.
Preferably, described full-automatic enclosed formula spraying freeze-drying production equipment also comprises clean water to introduce in closed container and cleans, and disinfectant is introduced the washing and sterilizing system of carrying out sterilizing in closed container, and described disinfectant can be sterile pure steam.
Preferably, described full-automatic enclosed formula spraying freeze-drying production equipment also comprises the control system for carrying out procedure auto-control to the freezing granulation of vacuum spraying and dynamic heat dry run, and described control system comprises at least one in programmable logic controller (PLC) (PLC) and computer (PC).
Present invention also offers a kind of full-automatic enclosed formula spraying freeze-drying production method, adopt above-mentioned full-automatic enclosed formula spraying freeze-drying production equipment, step is:
Step 1: selectively opened or close each valve of described equipment, utilizes vacuum system that closed container is extracted into certain vacuum;
Step 2: the freeze-drying atomization of liquid is separated into drop and sprays into cannon spray head to utilize atomizer to treat, the heat absorption of vaporizing in vacuum environment of constituent part in described drop makes drop temperature decline, described condensing unit is by the vacuum in the constituent part condensation in the drop described in after vaporization and then the container described in maintaining, and drop constant temperature declines until freeze to form ice particle;
Step 3: described ice granule materials is added in rotating cylinder by feed pipe; Dram temperature is controlled by temperature controlling circulating system; Rotating cylinder continues to rotate in dry run, and material rolls at cylinder bottom, contacts sufficiently uniformly be heated with barrel; Gathering sill rotates with rotating cylinder and is taken up from cylinder bottom by material, and material slides to discharging opening direction due to Action of Gravity Field on gathering sill, and when gathering sill continues to rotate with rotating cylinder, material falls bottom revolving drum due to Action of Gravity Field; By control spraying feeding quantity and rotating cylinder rotating speed make material with suitable speed to discharging opening move also uniformly dispersing at cylinder bottom, do not form accumulation, sublimation gases is discharged fast and to be taken away by vacuum system and to condense in condensing unit surface from material surface and particulate interspaces; Material continues the compound motion rolling and progressively move forward by drum rotation, dry gradually in rotating cylinder, until bone dry;
Step 4: dried material drops in discharging opening in rotating cylinder; When needing discharging, open top discharge valve, material falls into buffer area, closes top discharge valve, extraction valve; Open multiple pressure valve, pass into dried and clean aseptic gas to buffer area, make buffer area consistent with material collecting device inside and outside differential pressure; Open bottom discharge valve, collect dried material by material collecting device, close bottom discharge valve, multiple pressure valve after the emptying of buffer area material, open extraction valve, and change material collecting device; When needing discharging again, repeat this step.
Compared with prior art, the present invention has following beneficial effect:
1, by vacuum spraying freezing granulating technique, liquid is frozen into particle, drastically increase the freezing rate treating freeze-drying liquid, in cannon spray head, refrigerant nozzle is not set, in device, not there is liquid nitrogen cryogenics district, do not use refrigerant to contact with material in quick-frozen process completely, stop the contaminated risk of material completely, improve the aseptic of freeze-dry process, reduce energy consumption, and refrigerant recycles, do not produce to environmental emission and pollute.
2, make freeze-dried material dynamic overturn in rotating cylinder by rotary dryer, abundant, thermally equivalent, and sublimation gases is discharged fast, improve drying efficiency, shorten the drying time of material; Material main self gravitation that relies in heat drying apparatus carries out rolling or moving, and its original body state is protected; And dry run can be carried out continuously.
3, material after freeze-drying being transferred to normal pressure in vacuum tightness environment by Vacuum discharge mechanism, ensure that freeze-dry process can carry out continuously, protection closed container is not by environmental pollution.
4, whole freeze-drying produce in equipment keeping system airtight, from treating that freeze-drying liquid joins dried particles and releases, all reinforced, freeze dryings, discharging process are all carried out in sterile closed environment, reduce material by the risk of environmental pollution or contaminated environment; And whole process can be carried out continuously, ensure that the seal of freeze-dry process, aseptic and continuity.
5, compared to traditional freeze-drying explained hereafter process simplification, production efficiency improves, and automaticity improves, and energy consumption reduces, and equipment operation and maintenance cost reduces;
6, the scope of application is comparatively wide, and most injection and sterile bulk drug all can adopt this equipment to carry out freeze-drying, comprises and is much not suitable for using the protide preparation of traditional freeze dryer freeze-drying, biological products and poisonous, sensitization material etc.
Accompanying drawing explanation
Fig. 1 is the structural representation of traditional freeze drying plant;
The structural representation of the full-automatic enclosed formula spraying freeze-drying production equipment that Fig. 2 provides for embodiment 1;
Fig. 3 is the structural representation of the freezing prilling granulator of vacuum spraying in embodiment 1;
Fig. 4 is the structural representation of dynamic heat drying device in embodiment 1;
Fig. 5 is the structural representation of Vacuum discharge mechanism in embodiment 1;
The structural representation of the full-automatic enclosed formula spraying freeze-drying production equipment that Fig. 6 provides for embodiment 2;
Fig. 7 is the structural representation of the freezing prilling granulator of vacuum spraying in embodiment 2;
The structural representation of the full-automatic enclosed formula spraying freeze-drying production equipment that Fig. 8 provides for embodiment 3;
Fig. 9 is the structural representation of the freezing prilling granulator of vacuum spraying in embodiment 3;
Figure 10 is the structural representation of dynamic heat drying device in embodiment 4.
Detailed description of the invention
Below in conjunction with specific embodiment, set forth the present invention further.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.In addition should be understood that those skilled in the art can make various changes or modifications the present invention, and these equivalent form of values fall within the application's appended claims limited range equally after the content of having read the present invention's instruction.
Embodiment 1
The structural representation of the full-automatic enclosed formula spraying freeze-drying production equipment that Fig. 2 provides for the present embodiment, described equipment comprises the freezing prilling granulator 1 of the vacuum spraying being in turn connected to form closed container, dynamic heat drying device 2 and Vacuum discharge mechanism 3.
The structural representation of the freezing prilling granulator 1 of vacuum spraying that Fig. 3 provides for the present embodiment, described device comprises the cannon spray head 1-1 for holding product in mist projection granulating process; Multiple for treating that the freeze-drying atomization of liquid is separated into drop and sprays into the atomizer 1-2 in cannon spray head 1-1; For forming vacuum environment in closed container, the constituent part in described drop is vaporized heat absorption and then drop is lowered the temperature freeze to be formed the vacuum system of ice particle in this vacuum environment; And for by the condensing unit of constituent part condensation in the drop described in after vaporization.Described atomizer 1-2 is located in cannon spray head 1-1.Described vacuum system is connected with cannon spray head 1-1.
Described cannon spray head 1-1 top is tubular, and bottom is taper.Described condensing unit is the first refrigeration chuck 1-3 that the outside being located at cannon spray head 1-1 top passes into refrigerant, and refrigerant is silicone oil.Silicone oil is formed circulation by the fluid pump 1-4 on pipeline and is lowered the temperature by heat exchanger 1-5.The cross section of the first refrigeration chuck 1-3 is rectangle, arranges with the form of enclosing around the top one of cannon spray head 1-1.Be provided with the second refrigeration chuck 1-6 for avoiding ice particle to melt outside the lower taper of cannon spray head 1-1, passing into refrigerant in it is silicone oil.Silicone oil is formed circulation by the fluid pump 1-4 on another group pipeline and is lowered the temperature by heat exchanger 1-5.The cross section of the second refrigeration chuck 1-6 is rectangle, to arrange around the form of a circle outside cannon spray head 1-1 lower taper.Two described heat exchanger 1-5 connect refrigeration system 1-7.Described refrigeration system 1-7 is compressor.
Described atomizer 1-2 connects airtight dosing pipeline 1-8, passes into and treat freeze-drying liquid in pipeline, and dosing pipeline 1-8 is provided with flow control valve 1-9.Described vacuum system comprises vavuum pump 1-10, is connected by pipeline 1-11 with cannon spray head 1-1, and described pipeline 1-11 is provided with valve 1-12.The connector of cannon spray head 1-1 is provided with screen pack 1-13.
The bottom of described cannon spray head 1-1 is provided with the outlet valve 1-14 for releasing ice particle, and the outside of the roof of cannon spray head 1-1, upper portion side wall and lower sides is respectively provided with a vibrator 1-15 for ice particle is shaken off.Described vibrator 1-15 drives vibration by motor.Described outlet valve 1-14 is connected with dynamic heat drying device by pipeline.
The structural representation of the dynamic heat drying device 2 that Fig. 4 provides for the present embodiment, described device comprises: urceolus 2-1, feed pipe 2-2, discharging opening 2-4, and discharging opening has valve; Described cannon spray head 1-1 is connected with feed pipe 2-2 by outlet valve 1-14, and cannon spray head 1-1 and urceolus 2-1 forms closed container and protects container contents not by environmental pollution or contaminated environment; By rotating cylinder 2-11, rotating shaft 2-12, motor 2-13, and the rotary dryer of at least one axle bed composition, rotating cylinder 2-11 is used for holding and heat drying material, and rotating shaft 2-12 is used for motor 2-13 rotary power to pass to rotating cylinder 2-11; The temperature controlling circulating system be made up of swivel joint 2-21, heat exchanger 2-22, electric heater 2-23, fluid pump 2-24.
Be provided with at least one section of hollow jacket 2-15 outside rotating cylinder 2-11, every section of hollow jacket 2-15 is all by the expanding channels of pipeline and rotating shaft 2-12 inside, and a part that is whole, rotating shaft 2-12 of rotating cylinder 2-11 is arranged in closed container; Another part of rotating shaft 2-12 is connected with motor 2-13 outside closed container, and the inner passage of this part is connected with swivel joint 2-21; Described swivel joint 2-21 be side for being fixedly connected with, opposite side is used for connection rotating shaft 2-12 and carries fluid in its any rotation direction incessantly in continuous or discontinuous rotary motion, carries the device of electric current incessantly.Passing into fluid in described temperature controlling circulating system is silicone oil, and silicone oil is heated by electric heater 2-23 and regulates temperature by heat exchanger 2-22 and undertaken circulating by fluid pump 2-24 makes hollow jacket 2-15 barrel heat up or cooling.
The structural representation of the Vacuum discharge mechanism 3 that Fig. 5 provides for the present embodiment, described mechanism comprises the top discharge valve 3-1, the bottom discharge valve 3-2 that are located at below discharging opening 2-4, and two buffer area 3-3 between outlet valve, buffer area 3-3 is connected with closed container by the pipeline with extraction valve 3-5, and buffer area 3-3 also connects the pipeline passing into dried and clean aseptic gas with multiple pressure valve 3-6; Rewinding tank 3-4 is connected with bottom discharge valve 3-2.
Also can pass into clean water in the closed container of described equipment for cleaning container, disinfectant can be passed into for sterilizing containers, the preferred sterile steam of disinfectant.
When above-mentioned full-automatic enclosed formula spraying freeze-drying production equipment uses, treat that freeze-drying liquid can be normal-temperature water solution, suspension, emulsion etc., comprise or do not comprise auxiliary material, for the ivy powder aqueous solution by 125g ivy powder dissolution gained in 2L water, comprising the steps:
Step 1: first utilize vacuum system that the closed container that described cannon spray head 1-1 and urceolus 2-1 forms is extracted into negative pressure, vacuum is 300Pa.
Step 2: the first described refrigeration chuck 1-3 temperature controls as-60 DEG C, and the second refrigeration chuck 1-6 temperature controls as-20 DEG C, by dosing pipeline 1-8, described ivy powder aqueous solution is flowed to atomizer 1-2, atomisation pressure is 0.4MPa, nozzle diameter is 1.0mm, atomizer 1-2 is utilized the atomization of liquid to be separated into drop and to spray into cannon spray head 1-1, water in drop absorbs heat after vaporizing in vacuum environment and drop temperature is declined, vacuum system continues to vacuumize, water after vaporization is condensed in cannon spray head 1-1 inwall and then maintains vacuum by the first described refrigeration chuck 1-3, drop constant temperature declines until freeze to form ice particle, this process only needs the several seconds to complete, by the effect of vibration of vibrator 1-15 ice particle shaken off bottom cannon spray head 1-1 and release.Described drop does not directly contact with refrigerant and frozen in cannon spray head 1-1.
Step 3: the ice particle of material is joined in rotating cylinder 2-11 by feed pipe 2-2.It is 20 DEG C that described rotating cylinder 2-11 a certain section of hollow jacket 2-15 controls heating-up temperature by temperature controlling circulating system; Rotating cylinder 2-11 continues to rotate in dry run, and material rolls at cylinder bottom, contacts sufficiently uniformly be heated with barrel; Gathering sill 2-14 rotates with rotating cylinder and is taken up from cylinder bottom by material, material is slided to discharging opening 2-4 direction on gathering sill by Action of Gravity Field, gathering sill continues to rotate with rotating cylinder, material falls bottom revolving drum by Action of Gravity Field, by the Liquid addition of control flow check adjustable valve 1-9 and rotating cylinder rotating speed make material with suitable speed to discharging opening move and uniformly dispersing at cylinder bottom, do not form accumulation; Sublimation gases is discharged fast and to be taken away by vacuum system and to condense in cannon spray head 1-1 upper inside wall from material surface and particulate interspaces; Material is by the rolling of rotating cylinder rotation lasts with progressively to the compound motion of discharging opening migration, dry gradually in rotating cylinder, until bone dry.
Step 4: dried material drops in discharging opening 2-4 in rotating cylinder 2-11; When needing discharging, open top discharge valve 3-1, material falls in buffer area 3-3, closes top discharge valve 3-1, extraction valve 3-5; Open multiple pressure valve 3-6, pass into dried and clean aseptic gas to buffer area, make buffer area 3-3 consistent with material collecting device 3-4 inside and outside differential pressure; Open bottom discharge valve 3-2, collect dried material by material collecting device 3-4, close bottom discharge valve, multiple pressure valve in buffer area 3-3 after material emptying, open extraction valve, and change material collecting device; When needing discharging again, repeat this step.
Described full-automatic enclosed formula spraying freeze-drying production equipment carries out Automated condtrol by the control system be made up of programmable logic controller (PLC) and computer in freeze-drying process.
Embodiment 2
The structural representation of the full-automatic enclosed formula spraying freeze-drying production equipment that Fig. 6 provides for embodiment 2, the difference of this embodiment and embodiment 1 is the freezing prilling granulator part of vacuum spraying.
As shown in Figure 7, for the freezing prilling granulator structural representation of the vacuum spraying in embodiment 2, described device is similar to embodiment 1, difference is: described condensing unit is for being located at the outer and connected condenser 1-30 of cannon spray head 1-1, described condenser 1-30 connects the connector of cannon spray head 1-1 by pipeline 1-11, described vavuum pump 1-10 connects condenser 1-30 by another pipeline, the connecting pipe 1-11 of condenser 1-30 and cannon spray head 1-1 is provided with valve 1-12, and the outside on cannon spray head 1-1 top does not arrange the first refrigeration chuck 1-3.
For the ivy powder aqueous solution by 125g ivy powder dissolution gained in 2L water, when above-mentioned full-automatic enclosed formula spraying freeze-drying production equipment uses, implementation step is similar to embodiment 1, and difference is:
Step 2: in described liquid quick-frozen process, drop sprays into cannon spray head 1-1, water absorbs heat after vaporizing in vacuum environment and drop temperature is declined, vacuum system continues to vacuumize, described condenser 1-30 is by the water condensation after vaporization and then maintain vacuum in container, and drop constant temperature declines until freeze to form ice particle.
Step 3: described ice granule materials sublimation gases in heat drying process is discharged, and is taken away and condense on described condenser 1-30 by vacuum system.
Embodiment 3
The structural representation of the full-automatic enclosed formula spraying freeze-drying production equipment that Fig. 8 provides for embodiment 3, the difference of this embodiment and embodiment 1 is the freezing prilling granulator part of vacuum spraying.
As shown in Figure 9, for the freezing prilling granulator structural representation of the vacuum spraying in embodiment 3, described device is similar to embodiment 1, difference is: described condensing unit is the combination of the first refrigeration chuck 1-3 and condenser 1-30, the first described refrigeration chuck 1-3 is located at the outside on cannon spray head 1-1 top, and described condenser 1-30 is located at outside cannon spray head 1-1; Described condenser 1-30 connects the connector of cannon spray head 1-1 by pipeline 1-11, and described vavuum pump 1-10 connects condenser 1-30 by another pipeline, and the connecting pipe 1-11 of condenser 1-30 and cannon spray head 1-1 is provided with valve 1-12.
For the ivy powder aqueous solution by 125g ivy powder dissolution gained in 2L water, when above-mentioned full-automatic enclosed formula spraying freeze-drying production equipment uses, implementation step is similar to embodiment 1, and difference is:
Step 2: in described liquid quick-frozen process, drop sprays into cannon spray head 1-1, water absorbs heat after vaporizing in vacuum environment and drop temperature is declined, vacuum system continues to vacuumize, water after vaporization is condensed in cannon spray head 1-1 inwall by the first described refrigeration chuck 1-3, condenser 1-30 is by the water condensation after vaporization, and then vacuum in maintenance container, drop constant temperature declines until freeze to form particle.
Step 3: described ice granule materials sublimation gases in heat drying process is discharged, and is taken away and condense on described cannon spray head 1-1 upper inside wall and condenser 1-30 by vacuum system.
The cannon spray head 1-1 outside of the freezing prilling granulator of described vacuum spraying that the present embodiment provides connects multiple condenser 1-30, and described equipment continuous print carries out spraying freeze-drying and produces.
Embodiment 4
The structural representation of the full-automatic enclosed formula spraying freeze-drying production equipment that Fig. 2 provides for embodiment 4, composition graphs 5, Figure 10, the structure of the present embodiment can with embodiment 1,2,3 identical, implementation step is different.
For the ivy powder aqueous solution by 125g ivy powder dissolution gained in 2L water, when above-mentioned full-automatic enclosed formula spraying freeze-drying production equipment uses, the difference of implementation step is:
Step 2: in described liquid quick-frozen process, drop sprays into cannon spray head 1-1, stops spraying after freezing to form certain ice particle in batches.
Step 3: the material of glaciation particle is added in rotating cylinder 2-11 by feed pipe 2-2.In reinforced process, rotating cylinder 2-11 rotates, and material rolls at cylinder bottom, and now temperature controlling circulating system does not heat hollow jacket 2-15; Reinforced complete, temperature controlling circulating system starts heating, and rotating cylinder 2-11 reverses after driving rotating forward a period of time by motor 2-13, and switch through several times direction of rotation, material bilateral transfer in rotating cylinder is dry gradually; Until the material bone dry that this time adds.
Step 4: when needing discharging, open the multiple pressure valve 3-6 of Vacuum discharge mechanism, extraction valve 3-5 successively, dried and clean aseptic gas is passed in buffer area 3-3 and closed container, make the pressure of container consistent with material collecting device 3-4 pressure reduction, open top discharge valve 3-1, bottom discharge valve 3-2, discharging opening 2-4 and material collecting device 3-4 is connected, and rotating cylinder 2-11 rotates forward continuously until material is emptying.
The present embodiment uses full-automatic enclosed formula to spray the freeze-drying production material of freeze-drying production equipment batch.
Claims (10)
1. a full-automatic enclosed formula spraying freeze-drying production equipment, is characterized in that: comprise the freezing prilling granulator of vacuum spraying (1) and dynamic heat drying device (2) that are connected to each other composition closed container;
The freezing prilling granulator of vacuum spraying (1) comprises cannon spray head (1-1), be provided with for treating that the freeze-drying atomization of liquid is separated into the atomizer (1-2) of drop in described cannon spray head (1-1), described cannon spray head (1-1) connects and is used for being formed vacuum environment in closed container the constituent part in described drop vaporize heat absorption and then drop is lowered the temperature freeze the vacuum system of formation ice particle in this vacuum environment;
Dynamic heat drying device (2) comprises urceolus (2-1); Rotary dryer part for holding also heated material is located in urceolus (2-1); Temperature controlling circulating system for controlling rotary dryer heating-up temperature is connected with rotary dryer.
2. full-automatic enclosed formula spraying freeze-drying production equipment as claimed in claim 1, is characterized in that: the freezing prilling granulator of described vacuum spraying (1) also comprises for the condensing unit by the constituent part condensation in the drop described in after vaporization;
Described condensing unit is one in the first refrigeration chuck (1-3) and condenser (1-30) or its combination, the first described refrigeration chuck (1-3) is located at the outside on described cannon spray head (1-1) top, and the first refrigeration chuck (1-3) inside is connected with refrigerant; Described condenser (1-30) is located at described cannon spray head (1-1) outward, and is connected with described cannon spray head (1-1).
3. full-automatic enclosed formula spraying freeze-drying production equipment as claimed in claim 2, it is characterized in that: described vacuum system comprises vavuum pump (1-10), described cannon spray head (1-1) is provided with connector, and described connector is provided with valve; When described condensing unit is first refrigeration chuck (1-3), the connector of the cannon spray head (1-1) described in described vavuum pump (1-10) is connected by pipeline (1-11); When described condensing unit is the combination of condenser (1-30) or the first refrigeration chuck (1-3) and condenser (1-30), the connector of the cannon spray head (1-1) described in described condenser (1-30) is connected by pipeline (1-11), described vavuum pump (1-10) connects condenser (1-30) by another pipeline.
4. full-automatic enclosed formula spraying freeze-drying production equipment as claimed in claim 3, is characterized in that: the constituent part in described drop is water;
Described drop does not contact with refrigerant in described closed container;
The part that described cannon spray head (1-1) is described closed container; Described cannon spray head (1-1) top is tubular, and bottom is taper;
The outside of the bottom of described cannon spray head (1-1) is provided with the second refrigeration chuck (1-6) for avoiding ice particle to melt, and is connected with refrigerant in the second described refrigeration chuck (1-6);
The bottom of described cannon spray head (1-1) is provided with the tremie pipe (1-14) for releasing ice particle;
Described atomizer (1-2) connects airtight dosing pipeline (1-8), and described dosing pipeline (1-8) is provided with flow regulator (1-9).
5. full-automatic enclosed formula spraying freeze-drying production equipment as claimed in claim 4, it is characterized in that: the part that described urceolus (2-1) is described closed container, described urceolus (2-1) is provided with
For connecting the feed pipe (2-2) of the described tremie pipe (1-14) of the freezing prilling granulator of described vacuum spraying (1);
And the discharging opening (2-4) for releasing dried material.
6. full-automatic enclosed formula spraying freeze-drying production equipment as claimed in claim 1, is characterized in that: described rotary dryer comprises
For holding and the rotating cylinder (2-11) of heat drying material;
For the rotating shaft (2-12) that rotating cylinder (2-11) is connected with motor (2-13);
For giving the motor (2-13) of described rotating shaft (2-12) powered rotation.
7. full-automatic enclosed formula spraying freeze-drying production equipment as claimed in claim 6, it is characterized in that: a part that is whole, rotating shaft (2-12) for described rotating cylinder (2-11) is located in closed container, another part of described rotating shaft (2-12) is connected with described motor (2-13) outside closed container, is connected between described rotating shaft (2-12) with urceolus (2-1) by axle bed;
Described rotating cylinder (2-11) outside is provided with at least one section of hollow jacket (2-15), and in hollow jacket (2-15), through-flow body makes barrel heat up or cooling;
Described rotating cylinder (2-11) inwall be provided with at least one section with rotating cylinder rotation centerline gathering sill at an angle (2-14), when rotating cylinder (2-11) rotates forward, material is directed to groove (2-14) and is with trend discharging opening direction to move; When rotating cylinder (2-11) reversely rotates, material is brought back.
8. full-automatic enclosed formula spraying freeze-drying production equipment as claimed in claim 7, it is characterized in that: described temperature controlling circulating system comprises the swivel joint (2-21), heat exchanger (2-22), electric heater (2-23) and the fluid pump (2-24) that connect to form a closed-loop path successively, logical circulation of fluid in closed-loop path;
Described rotating shaft (2-12) inside is provided with the passage for fluid circulation, and this passage side is connected with one or more snippets hollow jacket (2-15) on described rotating cylinder (2-11) in described closed container; This passage opposite side is connected with described swivel joint (2-21) outside closed container; Described swivel joint (2-21), in rotating shaft (2-12) the arbitrarily continuous or discontinuous rotary motion of rotation direction, makes the fluid in described closed-loop path carry incessantly in described hollow jacket (2-15);
The detector for detecting material information is provided with in described rotating cylinder (2-11), described detector is connected with described swivel joint (2-21), and described swivel joint (2-21) carries electric current incessantly in rotating shaft (2-12) the arbitrarily continuous or discontinuous rotary motion of rotation direction.
9. full-automatic enclosed formula spraying freeze-drying production equipment as claimed in claim 8, is characterized in that: also comprise for being released in vacuum airtight container by dried material, returns to packing under atmospheric pressure and the Vacuum discharge mechanism (3) of rewinding;
Described Vacuum discharge mechanism (3) comprises top discharge valve (3-1), the bottom discharge valve (3-2) of being located at described dynamic heat drying device (2) discharging opening (2-4) below, buffer area (3-3) is provided with between top discharge valve (3-1), bottom discharge valve (3-2), buffer area (3-3) is connected with the urceolus of described dynamic heat drying device (2) by the pipeline being provided with extraction valve (3-5), and the dried and clean aseptic gas that buffer area (3-3) is also connected with multiple pressure valve (3-6) passes into pipeline; Material collecting device (3-4) is connected with bottom discharge valve (3-2).
10. a full-automatic enclosed formula spraying freeze-drying production method, is characterized in that, adopt full-automatic enclosed formula spraying freeze-drying production equipment as claimed in claim 9, step is:
Step 1: selectively opened or close each valve of described equipment, utilizes vacuum system that the closed container that freezing for vacuum spraying prilling granulator (1) and dynamic heat drying device (2) are connected to each other composition is extracted into certain vacuum;
Step 2: the freeze-drying atomization of liquid is separated into drop and sprays into cannon spray head (1-1) to utilize atomizer (1-2) to treat, the heat absorption of vaporizing in vacuum environment of constituent part in described drop makes drop temperature decline, described condensing unit by vaporization after described in drop in constituent part condensation so that maintain described in closed container in vacuum, drop constant temperature decline until freeze formed particle;
Step 3: described ice granule materials is added in rotating cylinder (2-11) by feed pipe (2-2); Rotating cylinder (2-11) temperature is controlled by temperature controlling circulating system; Rotating cylinder (2-11) continues to rotate in dry run, and material, in the rolling of rotating cylinder (2-11) bottom, contacts with barrel sufficiently uniformly and is heated; Gathering sill (2-14) rotates with rotating cylinder (2-11) and is taken up from rotating cylinder (2-11) bottom by material, material slides to discharging opening (2-4) direction due to Action of Gravity Field on gathering sill (2-14), when gathering sill (2-14) with rotating cylinder continue rotate, material due to Action of Gravity Field fall revolving drum (2-11) bottom; By control spraying feeding quantity and rotating cylinder (2-11) rotating speed make material with suitable speed to discharging (2-4) move also uniformly dispersing at cylinder bottom, do not form accumulation, sublimation gases is discharged fast and to be taken away by vacuum system and to condense in condensing unit surface from material surface and particulate interspaces, material rotates the compound motion continuing rolling and progressively move forward by rotating cylinder (2-11), dry gradually in rotating cylinder (2-11), until bone dry;
Step 4: dried material drops in discharging opening (2-4) in rotating cylinder (2-11); When needing discharging, open top discharge valve (3-1), material falls into buffer area (3-3), closes top discharge valve (3-1), extraction valve (3-5); Open multiple pressure valve (3-6), pass into dried and clean aseptic gas to buffer area, make buffer area (3-3) consistent with material collecting device (3-4) inside and outside differential pressure; Open bottom discharge valve (3-2), dried material is collected by material collecting device (3-4), bottom discharge valve (3-2), multiple pressure valve (3-6) is closed after the emptying of buffer area (3-3) material, open extraction valve (3-5), and change material collecting device (3-4); When needing discharging again, repeat step 4.
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| CN201510790555.5A CN105318665B (en) | 2015-11-17 | 2015-11-17 | A kind of full-automatic enclosed formula spraying freeze-drying production equipment and method |
| PCT/CN2015/098807 WO2017084162A1 (en) | 2015-11-17 | 2015-12-24 | Full-automatic sealed-type spray-freeze-drying production equipment and method |
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| CN201510790555.5A CN105318665B (en) | 2015-11-17 | 2015-11-17 | A kind of full-automatic enclosed formula spraying freeze-drying production equipment and method |
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| CN105318665B (en) | 2018-06-29 |
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