EP3775739B1 - Gefriertrocknungsanlage und verfahren hierzu - Google Patents

Gefriertrocknungsanlage und verfahren hierzu Download PDF

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Publication number
EP3775739B1
EP3775739B1 EP18822285.5A EP18822285A EP3775739B1 EP 3775739 B1 EP3775739 B1 EP 3775739B1 EP 18822285 A EP18822285 A EP 18822285A EP 3775739 B1 EP3775739 B1 EP 3775739B1
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EP
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Prior art keywords
sound
drying
freeze
product
fluid
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EP18822285.5A
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German (de)
English (en)
French (fr)
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EP3775739A1 (de
Inventor
Torsten PÄCHNATZ
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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
    • F26B23/00—Heating arrangements
    • F26B23/10—Heating arrangements using tubes or passages containing heated fluids, e.g. acting as radiative elements; Closed-loop systems
    • 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
    • F26B5/02—Drying solid materials or objects by processes not involving the application of heat by using ultrasonic vibrations
    • 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
    • F26B5/044—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 for drying materials in a batch operation in an enclosure having a plurality of shelves which may be heated

Definitions

  • the invention relates to a freeze-drying system for drying liquid-containing, ie generally solvent-containing products, and the invention relates to a method for drying such products with such a freeze-drying system.
  • the freeze-drying system is designed with a vacuum chamber, in which at least one receiving device for receiving the products is introduced, and at least one sound generator is arranged on the receiving device, with which the product can be sonicated during the drying phase.
  • Freeze drying which is known per se, is a process for the gentle evaporation of a wide variety of solvents that are present, for example, in foods, in medicines and the like as a result of production or are naturally present.
  • Freeze-drying equipment is used to carry out the freeze-drying process, and the drying takes place through the evaporation of the solvent in the product itself.
  • the solvent and thus the frozen liquid go directly and without prior transition to the liquid phase from the frozen to the gaseous state, which is called called sublimation.
  • sublimation By creating a vacuum, the liquid can already be sublimated at significantly lower temperatures, so that the product is not subjected to high thermal loads.
  • the low thermal stress enables the properties of the product to be retained, for example the preservation of oils, aromas and other preferably taste-related properties, as well as the consistency of the product.
  • freeze-drying A well-known example of the use of freeze-drying is the production of so-called instant coffee, which is produced using freeze-drying, in particular in order to preserve the aromatic substances in the soluble coffee for later enjoyment.
  • instant coffee which is produced using freeze-drying, in particular in order to preserve the aromatic substances in the soluble coffee for later enjoyment.
  • the excellent solubility of the freeze-dried product with the liquid still removed and storage at room temperature are particularly advantageous.
  • Freeze-drying systems usually have a vacuum chamber for receiving the products, for which coolable and heatable shelves are accommodated in the vacuum chamber, and a condenser is provided, which is usually in a separable from the receiving space Capacitor chamber is housed.
  • the product is first frozen, kept frozen and placed in the vacuum chamber, which is then closed and evacuated.
  • the product is then heated under the created vacuum and the sublimation energy consumed in the course of drying is fed back.
  • the condenser is cooled to low temperatures with a refrigeration unit, in particular with a refrigerant, in order to recondense the liquid from the vapor phase that has sublimated from the product on the surface of the condenser.
  • freeze-drying is divided into three sub-steps that are separated in terms of time, namely freezing, main drying and post-drying.
  • the vacuum is created and the pressure is reduced to a value that is below the freezing point of the liquid in the phase diagram.
  • the pressure value to be set depends essentially on the liquid temperature to be maintained and is determined using the vapor pressure curve.
  • the actual drying process takes place exclusively through the sublimation of liquid in the product under the set pressure vacuum.
  • the sublimation energy used in the main drying to remove the liquid from the product is returned to the product in the receiving device in the form of heat.
  • receiving devices generally have receiving plates and a line device, and a fluid can be guided through corresponding fluid channels in the receiving plate via the line device. Silicone oil, for example, is used as the fluid.
  • Silicone oil for example, is used as the fluid.
  • the layer thickness of the dried product also increases from the outside in and the rate of sublimation increases.
  • the shelf temperature on the top of the receiving plates is continuously increased, but the maximum temperature is limited in order not to damage the product, in particular to prevent the product from defrosting.
  • Known freeze-drying systems are constructed in such a way that the vacuum chamber is separated from the condenser chamber by a dividing wall, for example, or has some other separation from the condenser chamber, and the vacuum chamber is connected to the condenser chamber via an openable valve, which is introduced, for example, in the dividing wall.
  • the valve is opened and the solvent vapor, for example water vapor, can pass into the condenser chamber and condense on the surface of the condenser.
  • the capacitors consist for example from cooling coils and are cooled to low temperatures with a refrigerant via a compressor.
  • the vacuum chamber and usually also the condenser chamber are vented to normal pressure again.
  • a vacuum connection via which the vacuum chamber and/or the condenser chamber can be connected to an external compressor, is used to aerate the vacuum chamber and/or the condenser chamber.
  • FIG. 1 a freeze-drying system 1 according to the prior art for drying liquid-containing products 10.
  • the freeze-drying system 1 has a vacuum chamber 11 and a condenser chamber 25, which is separated from the vacuum chamber 11 by an intermediate wall 21, for example.
  • a receiving space 15 is formed in the vacuum chamber 11, in which a receiving device 12 for receiving the product 10 is introduced.
  • the receiving device 12 has a plurality of receiving plates 16, and the receiving device 12 comprises a line device 19 with a number of fluid lines 24.
  • a condenser 13 is placed in the condenser chamber 25 and the condenser chamber 25 can be connected to the receiving space 15 of the vacuum chamber 11 by opening a valve 22 in the intermediate wall 21 .
  • the products 10 are placed on the receiving plates 16 in the frozen state.
  • the vacuum chamber 11 is then closed and a negative pressure is generated in the vacuum chamber 11 .
  • Sublimation then begins, with the temperature of the product 10 increasing as the degree of drying increases.
  • the line device 19 with the fluid lines 24, through which a fluid 20, for example silicone oil, is guided serves for this purpose can.
  • the fluid 20 which can be temperature-controlled outside of the vacuum chamber 11, the installation surfaces on the capacitor plates 16 and thus also the products 10 can be heated accordingly.
  • the temperature above the fluid 20 in the products 10 is also increased, with the valve 22 being opened as the vapor pressure in the receiving space 15 increases, and the vapor phase of the liquid, for example water vapor or solvent vapor in general, can reach the surface of the condenser 13 condense.
  • the atmosphere in the receiving space 15 is exchanged with the atmosphere in the condenser chamber 25. If the drying has also taken place with the further post-drying phase while at the same time further heating of the products 10, the vacuum connection 26 is opened and the receiving space is opened at the same time as the valve 22 15 and the condenser chamber 25 is ventilated again. The dried product 10 can then be removed.
  • the receiving device 12 can have a plurality of receiving plates 16 which are arranged one above the other and whose distance from one another can be changed by a corresponding actuator system. In this way, vessels for pharmaceutical products, for example, can be automatically sealed after drying, in particular in order to provide the dried product 10 aseptically.
  • the GB 948 517 A a grinding or granulating the product 10 before, and the ground or granulated product, such as instant coffee, is guided over vibrating receiving plates so that the product to be dried during the Drying phase remains in motion, in particular to effectively use a large surface of the ground or granulated product for drying.
  • grinding or granulating a product is not possible for every product, and there are products, such as medicines, that have to be applied to the receiving plates of the receiving device in magazine form in containers and, for example, have a powder-like consistency that is still bound with solvent.
  • the use of ultrasound to improve the drying process in freeze-drying systems is known.
  • the influence of ultrasound on the product improves the permeability of the product to be dried, so that the liquid can also sublimate better from the inner areas of the product.
  • the influence of ultrasound on the mass transport process when drying the products is based on minimizing internal and external resistances for heat and mass transport, so that the diffusion barriers are reduced and the formation of boundary layers is mitigated.
  • the implosion of gas bubbles known as cavitation and caused by the cyclic alternating pressure and the resulting microflows can also influence interfaces and thus reduce external resistance to mass transport in the product and mass transfer at the product surface.
  • Ultrasound is intended to accompany the drying of the product during the drying phase. Further details can be found in AiF 17161 N; "Improvement of drying processes of vegetable raw materials by process-induced reduction of mass transport resistances"; Food Industry Research Group (FEI), Bonn.
  • the sonication of the product with ultrasound usually takes place with a sound generator arranged outside of the vacuum chamber, so that the targeted influence of the ultrasound on the product can only be achieved to a limited extent.
  • a sound generator arranged outside of the vacuum chamber, so that the targeted influence of the ultrasound on the product can only be achieved to a limited extent.
  • the ultrasound is usually no longer used as an accompaniment to this.
  • the JP S61 178 185 U and the JP S63 132 292 U each disclose a freeze-drying plant for drying liquid-containing products, and a vacuum chamber is shown in which receiving devices for receiving the liquid-containing products are introduced.
  • the freeze-drying system also has a sound generator, which is arranged on the receiving device and with which the product can be exposed to sound during the drying phase.
  • the EP 3 093 597 A1 discloses a further embodiment of a freeze-drying system for drying liquid-containing products, with no sound generator being disclosed which is intended to transmit sound waves into the product to be dried.
  • pamphlet CN 103 968 649 A discloses a further embodiment of a freeze-drying system for drying liquid-containing products, an ultrasonic generator with a plurality of ultrasonic heads being provided, and the ultrasonic heads being arranged on a receiving device on which, for example, vegetables intended for freeze-drying can be placed.
  • the ultrasound head can be used directly mechanical vibration transmission arranged on the receiving plate.
  • GB 2 400 901A yet another embodiment of a freeze-drying system with a vacuum chamber and with a sound generator for sounding in ultrasound, the ultrasound being applied while the products are being frozen, so that a crystal structure that is as fine as possible is formed in the frozen product.
  • This improves the actual drying process in a manner known per se, although the actual drying process is not accompanied by the action of ultrasound.
  • the object of the invention is to improve a freeze-drying installation for drying liquid-containing products and to improve a method for drying liquid-containing products using such a freeze-drying installation.
  • the use of ultrasound as a supporting means in the drying of liquid-containing products should be used in an improved manner, preferably in order to accelerate the drying process and, as a result, to achieve a simpler construction of the freeze-drying system.
  • the invention provides that there is a condenser that can be cooled, on which liquid extracted from the product in a drying phase can be condensed from a vapor phase, and that the receiving device comprises a line device for passing a fluid through, with the sound generator on the line device is arranged and that the sound generator is designed to turn on a sound in the fluid.
  • the receiving device can have one or more receiving plates, whereby the invention is also based on the idea that the receiving device can also include a line device and other structural parts, for example, through which a fluid can be passed, in particular in order to cool or seal the receiving plates heat.
  • the receiving device in the sense of the invention can include several tiers for placing the products, or the receiving device is designed in several parts and has a base plate on which one or more trays are arranged, in which the products lie.
  • the products can relate to medicines or food, for example, which is particularly isolated and unpackaged on the
  • Mounting plate so rest at least indirectly.
  • the receiving space is formed in the vacuum chamber, in which the receiving device with the product or products is located, wherein as a further aspect of the invention the condenser can also be accommodated in the receiving space.
  • the vacuum chamber thus forms a single receiving space, in which both the receiving device with the product or products and at the same time with the condenser are accommodated, which simplifies the structure of the system. Consequently, the intermediate wall with the valve can be omitted, whereby only a vacuum connection for evacuation and ventilation can be present, over which the vacuum can be maintained with the required pressure values, especially if a corresponding compressor is attached to the vacuum connection.
  • the invention is also directed to freeze-drying systems which have a condenser chamber which can only be connected to the vacuum chamber by opening a valve.
  • the basic idea of the invention is particularly reflected in the fact that the sound generators radiate at least indirectly into the receiving plates in such a way that the solid-state sound in the receiving plate can be transferred to the product.
  • the recording plate is multi-part, and the sound is transferred from body to body of the multi-part recording plate. Such a transfer can take place in particular from the receiving plate into a receiving dish or other receiving vessel for receiving the product.
  • sound generators refer to all technical devices that are suitable for introducing sound, in particular ultrasound, into a substance, ie a liquid or a solid, and causing this or this to vibrate.
  • the sound generator can also be in several parts and only one sonotrode is arranged on the receiving device and a corresponding generator, which is connected to the sonotrode comprising the exciter only by means of an electrical line.
  • the generator does not also have to be arranged in the receiving space of the vacuum chamber, since it is sufficient for the sonotrode with the sound exciter to be arranged on the receiving device.
  • Sound generators and thus the part of the sound generator that can be arranged on the receiving device according to the invention can be designed as cuboids, discs, cylinders or other components that can be easily attached to the receiving device with dimensions of, for example, a few centimeters.
  • the sound generators are designed as round or square disks or plates that have lateral dimensions that correspond approximately to the installation dimensions of the containers in which the products are accommodated.
  • the condenser of the freeze-drying system is designed with particular advantage as a cooling coil and has a pipe or is formed by a pipe through which a refrigerant is passed when the freeze-drying system is in operation and the condenser is cooled.
  • the condenser in particular in the form of the cooling coil, can be designed spatially in such a way that it encloses the receiving device on the outside.
  • a compact design can be achieved if, according to a possible embodiment, both the receiving device with the products the condenser are also accommodated in a common accommodation space of the vacuum chamber.
  • the receiving device comprises a receiving plate which is formed by means of a bottom sheet of the vacuum chamber.
  • the receiving device has a line device for the passage of a fluid, it being possible for the sound generator to also be arranged on the line device in order to inject sound into the fluid.
  • the sound from the sound generator can be brought to the receiving plate via the fluid and thus via the fluid column, in order finally to radiate sound into the product that is placed on the receiving plate.
  • the sound generator forms an ultrasonic generator and this generates a sound with a sound frequency of at least 16 kHz, for example up to 1 GHz.
  • the sound is conducted to the product by means of solid-state sound transmission in the receiving plate and/or via a fluid column of the fluid in the fluid line and finally radiated into the product.
  • sound can be injected into the fluid line and thus into the fluid column, which can then be transferred to the receiving plate and can finally reach the product from there.
  • the object of the invention is also achieved by a method for drying liquid-containing products with a freeze-drying system, the method comprising at least the following steps: arranging at least one sound generator on a receiving device for receiving the liquid-containing products in the vacuum chamber and sonicating the product during the drying phase by means of a sound wave line through at least part of the recording device with the sound generator.
  • the receiving device is designed with a line device for carrying a fluid through, with the sound generator being arranged on the line device and injecting sound into the fluid, so that the sound is guided through the fluid to the receiving plate and thus to the product.
  • the receiving device with the product(s) and a condenser of the freeze-drying system can be accommodated separately from one another in separate chambers or in a common accommodation space only in the vacuum chamber. This eliminates a valve, in particular in an intermediate wall, to form a connection to the condenser space in which the condenser is arranged. Due to the influence of the ultrasound during operation of the ultrasonic generator, the drying process is accelerated to such an extent that a single cycle can suffice to completely dry the product.
  • the influence of the ultrasound in particular by selecting a correspondingly higher power of the ultrasound generator, only has to be conducted to a lesser extent via the fluid heat to the product, with a possible further development of a freeze-drying system and an associated method being aligned in this way according to the invention It may be that the product is heated up entirely by the influence of the ultrasound, especially if the sound generators are operated at higher power.
  • the line device with the fluid lines and the heating and cooling fluid can thus also be omitted, which further simplifies the design of the freeze-drying system and the execution of the method.
  • FIG. 1 1 shows a freeze-drying plant 1 according to the prior art, and the freeze-drying plant 1 has already been dealt with in detail in connection with the introductory part of the present description.
  • FIG. 1 shows a freeze-drying plant 1 which is not part of the invention, and the freeze-drying plant 1 has a Vacuum chamber 11, and the vacuum chamber 11 forms a receiving space 15 that can be evacuated.
  • a receiving device 12 for receiving products 10 to be dried is received.
  • a condenser 13 is located in the same receiving space 15 and, for example, encloses the receiving device 12 on the outside.
  • the receiving device 12 has a plurality of receiving plates 16 on which the products 10 to be dried are placed.
  • a line device 19 with fluid lines 24 is connected to the receiving plates 16 and a fluid 20 , for example a silicone oil, can be passed through the fluid lines 24 .
  • the fluid 20 can be cooled or heated with peripheral devices, so that the products 10 can also be cooled and in particular heated via the heat exchange with the receiving plates 16 .
  • the receiving plates 16 below the receiving plates 16 are several sound generators 14 for emitting a sound, in particular an ultrasound, so that the direct arrangement of the sound generators 14 on the receiving plates 16 the products 10 placed on the receiving plates 16 can be exposed to sound directly.
  • a sound in particular an ultrasound
  • the vacuum chamber 11 has a vacuum connection 26, via which the vacuum chamber 11 can be evacuated or vented again with the aid of other peripheral devices (not shown).
  • the products 10 can first be placed or placed in the receiving device 12 in the frozen state or introduced into the vacuum chamber 11 together with the receiving device 12 .
  • the vacuum chamber 11 is then closed and evacuated via the vacuum connection 26 .
  • the falling phase transition point from the solid phase of the liquid in the frozen product allows it to go directly to the vapor state without forming a liquid phase, causing the product 10 to dry.
  • a coolant flows through the condenser 13, it can be brought to a very low freezing temperature, and the liquid vapor from the sublimation process of the product 10 can condense directly on the surface of the condenser 13.
  • the sound generators 14 are operated during the drying phase of the products 10 and the sound generators transmit, for example, ultrasound directly into the products 10, the sublimation of the liquid in the products 10 is significantly accelerated.
  • the temperature of the product 10 can be uniformly increased by the action of ultrasound, so that the associated heating can take place in addition to or as an alternative to heating the products 10 via a heated fluid 20.
  • the condensers can also be equipped with sound generators and sonicated in order to achieve a higher packing density of the precipitating ice from the gas phase of the liquid through the effect of the sound excitation, since smaller ice crystals are formed.
  • FIG. 12 shows, by way of example, an enlarged view of the product 10 which is placed on an upper side 17 of the receiving plate 16.
  • FIG. A sound generator 14 is arranged on the underside 18 of the receiving plate 16 and can transmit sound, in particular ultrasound, directly through the receiving plate 16 into the product 10 .
  • the product 10 can be stored in a container and on the Top 17 of the receiving plate 16 stand up. If several products 10 are set up on the receiving plate 16, several sound generators 14 assigned to the respective products 10 can also be arranged on the underside 18 of the receiving plate 16.
  • figure 4 12 shows an alternative embodiment of the receiving device 12, and a receiving plate 16 mounted on a frame 29 is shown, and a plurality of products 10 are standing on the upper side 17 of the receiving plate 16.
  • a sound generator 14 is arranged on the underside 18 of the mounting plate 16 .
  • the example according to figure 4 also shows the possibility that a base plate 16' of the vacuum chamber 11 forms the receiving device 12 for receiving the products 10, and the sound generator 14 is arranged on the outside under the base plate 16'.
  • the base plate 16' thus forms an alternative form of the receiving plate 16 and thus also a part of the receiving device 12.
  • figure 5 represents an embodiment of the freeze-drying system 1 according to the invention, with a vacuum chamber 11 in which the receiving space 15 is formed, and in the receiving space 15 the receiving device 12 has been introduced.
  • the receiving device 12 in turn has a plurality of receiving plates 16 and each of the receiving plates 16 is connected with individual lines to the line device 19 which comprises a number of fluid lines 24 through the passage of the fluid 20 .
  • the condenser 13 is also arranged in the vacuum chamber 11 and the vacuum chamber 11 has a vacuum connection 26 for evacuation and ventilation of the same.
  • the products 10 are placed on top of the receiving plates 16, with six products 10 being shown as an example.
  • a sound generator 14 is arranged on a fluid line 24 and can introduce sound, in particular ultrasound, into the line device 19 .
  • the sound is conducted via the fluid line itself, but in particular also via the fluid column which is guided into the receiving plates 16, see for example a fluid flow arrow in front of the second receiving plate 16 on which the products 10 are placed.
  • This makes use of the possibility of introducing an ultrasound into all receiving plates 16 with a centrally arranged sound generator and the line branching of the line device 19, which can be brought directly to the products 10 via the line and in particular via the liquid column, which are on the upper side of the receiving plates 16 are set up.
  • An alternative sounding point 28 can be formed, for example, in or on each of the fluid lines 24, at which a sound generator is arranged for each mounting plate 16.
  • figure 6 shows a detailed view of a receiving plate 16, and in the receiving plate 16 there is a fluid channel 27 through which the fluid 20 is guided and which is connected to the fluid line 24.
  • a fluid channel 27 through which the fluid 20 is guided and which is connected to the fluid line 24.
  • On the top 17 of the receiving plate 16 is an example of a product 10 on.
  • a sound generator 14 is arranged on one end side of a section of the fluid line 24 extending in a straight line, which can insonate a sound, in particular ultrasound, into the area of the fluid 20 that flows through the fluid channel 27 within the receiving plate 16 .
  • the schematic view illustrates the possibility of using the fluid column of the fluid to bring the sound to the product 10, and the fluid can be used at the same time as a heating and cooling fluid for heating and cooling the product 10.

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  • Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Mechanical Engineering (AREA)
  • General Engineering & Computer Science (AREA)
  • Health & Medical Sciences (AREA)
  • Molecular Biology (AREA)
  • Chemical & Material Sciences (AREA)
  • Combustion & Propulsion (AREA)
  • Sustainable Development (AREA)
  • Drying Of Solid Materials (AREA)
EP18822285.5A 2018-04-05 2018-12-06 Gefriertrocknungsanlage und verfahren hierzu Active EP3775739B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102018002776 2018-04-05
PCT/EP2018/083783 WO2019192747A1 (de) 2018-04-05 2018-12-06 Gefriertrocknungsanlage und verfahren hierzu

Publications (2)

Publication Number Publication Date
EP3775739A1 EP3775739A1 (de) 2021-02-17
EP3775739B1 true EP3775739B1 (de) 2022-08-24

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Country Status (7)

Country Link
US (1) US11473839B2 (zh)
EP (1) EP3775739B1 (zh)
JP (1) JP7071582B2 (zh)
CN (1) CN111971519A (zh)
ES (1) ES2926689T3 (zh)
PT (1) PT3775739T (zh)
WO (1) WO2019192747A1 (zh)

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PT3775739T (pt) * 2018-04-05 2022-09-28 Paechnatz Torsten Sistema de liofilização e processo para o mesmo
DE202021101537U1 (de) * 2021-03-24 2021-05-18 Torsten Pächnatz Gefriertrocknungsanlage
CN114485077B (zh) * 2022-02-23 2024-06-25 上海理工大学 一种超声辅助冷冻干燥设备
CN115574547B (zh) * 2022-02-23 2023-12-01 上海理工大学 一种超声辅助冷冻干燥方法
CN116182522B (zh) * 2023-04-18 2024-09-17 烟台冰轮冻干智能科技有限公司 一种食品真空冷冻加热板组及其干燥机

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EP3172515B1 (en) * 2014-07-24 2021-07-14 Heat Technologies, Inc. Acoustic-assisted heat and mass transfer device
EP3093597B1 (de) 2015-05-11 2017-12-27 Martin Christ Gefriertrocknungsanlagen GmbH Gefriertrocknungsanlage
TWI580918B (zh) * 2015-10-29 2017-05-01 Tai Yiaeh Enterprise Co Ltd The immediate detection method of the drying process
PT3775739T (pt) * 2018-04-05 2022-09-28 Paechnatz Torsten Sistema de liofilização e processo para o mesmo
CN111041055A (zh) * 2019-12-12 2020-04-21 江苏大学 超声协同普鲁兰酶制备慈姑抗性淀粉方法
JP2023514540A (ja) * 2020-02-04 2023-04-06 リジェネロン・ファーマシューティカルズ・インコーポレイテッド 凍結乾燥医薬品の目標残留水分含有量

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WO2019192747A1 (de) 2019-10-10
ES2926689T3 (es) 2022-10-27
PT3775739T (pt) 2022-09-28
US11473839B2 (en) 2022-10-18
JP2021519914A (ja) 2021-08-12
CN111971519A (zh) 2020-11-20
JP7071582B2 (ja) 2022-05-19
US20210172679A1 (en) 2021-06-10

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