EP0301117A1 - Freeze-drying apparatus - Google Patents

Freeze-drying apparatus Download PDF

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Publication number
EP0301117A1
EP0301117A1 EP87110955A EP87110955A EP0301117A1 EP 0301117 A1 EP0301117 A1 EP 0301117A1 EP 87110955 A EP87110955 A EP 87110955A EP 87110955 A EP87110955 A EP 87110955A EP 0301117 A1 EP0301117 A1 EP 0301117A1
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EP
European Patent Office
Prior art keywords
valve
condensation surface
refrigerant
condenser
freeze
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Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
EP87110955A
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German (de)
French (fr)
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EP0301117B1 (en
Inventor
Heinrich Steinkamp
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
GEA Lyophil GmbH
Original Assignee
Leybold AG
Amsco Finn Aqua GmbH
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Application filed by Leybold AG, Amsco Finn Aqua GmbH filed Critical Leybold AG
Priority to EP87110955A priority Critical patent/EP0301117B1/en
Priority to DE3750847T priority patent/DE3750847D1/en
Priority to ES87110955T priority patent/ES2068809T3/en
Priority to JP63173852A priority patent/JP2676374B2/en
Priority to US07/226,536 priority patent/US4949473A/en
Publication of EP0301117A1 publication Critical patent/EP0301117A1/en
Application granted granted Critical
Publication of EP0301117B1 publication Critical patent/EP0301117B1/en
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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

Definitions

  • the present invention relates to a device for freeze drying with an evacuable chamber and an evacuation system.
  • Freeze drying is primarily used to preserve temperature-sensitive products, the properties of which should be retained. Freeze-drying is mainly used in the fields of pharmacy, biology and medicine.
  • the usual freeze-drying process takes place approximately as follows: after freezing the product containing water, the sublimation of the water in ice form takes place under vacuum (about 10uum1 mbar). After this main drying, the post-drying takes place, during which the adsorptively bound moisture is removed in order to achieve extremely low residual moisture. During the final drying, the product is warmed up in compliance with permissible temperature limits. The pressure at which post-drying takes place is around 10 ⁇ 3 mbar.
  • the present invention has for its object to provide a freeze-drying device of the type mentioned, in which the product batches are no longer at risk from accidents of the type described or a similar type.
  • this object is achieved in that the device is additionally equipped with a condensation surface which is connected to a valve Storage container with a low-boiling refrigerant is connected.
  • the valve between the further condensation surface in the condenser and the storage container is opened so that the refrigerant flows into the condensation surface.
  • the further condensation surface thus takes over the pumping effect.
  • the vacuum in the freeze-drying chamber remains independent of the equipment, so that there is no risk of thawing or thawing of the product.
  • the additional condensation surface can be accommodated in the freeze-drying chamber, in the condenser that is usually connected to the freeze-drying chamber, or in a separate chamber.
  • the device for freeze drying shown in the figure comprises the vacuum chamber 1 with the shelves 2 on which the product is located during the course of the freeze drying process.
  • the shelves 2 are usually both coolable and heatable.
  • the shelves 2 are equipped with cavities, not shown in detail, through which a temperature control agent (for example silicone oil) flows.
  • the temperature control circuit is shown in dash-dot lines and labeled 3.
  • the setting plates 2 are parallel to each other and the feed pump 4 is switched on. If the circulating refrigerant is to be cooled, then the compressor refrigeration machine 5 is started up.
  • the compressor refrigeration machine 5 is located in the refrigerant circuit 6, which usually comprises the water-cooled condenser 7, the heat exchanger 8 and the valve 9.
  • the condenser 7 is preferably water-cooled.
  • the heat exchanger 8 is in the Temperature control circuit 3 switched on. Often, several compressor chillers are used at this point in order to either ensure operation (separate circuits) or to reach lower temperatures (cascade connection). Another chiller (e.g. adsorption chiller) can also be used.
  • the heating of the setting plates 2 is usually carried out by means of an electrical heating, not shown in detail, of the temperature control medium circulating in the temperature control circuit 3.
  • an electrical heating not shown in detail
  • the use of waste heat from the chillers or the use of steam-heated heat exchangers is also possible.
  • An evacuation system 11 is connected to the vacuum chamber 1 and comprises a condenser 12 and a vacuum pump 13 (gas ballast pump).
  • the valve 15 is located in the connecting line 14 between the vacuum chamber 1 and the condenser 12.
  • the line 16 with the valve 17 extends between the condenser 12 and the vacuum pump 13.
  • condensation surfaces 18 are accommodated within the condenser 12 and serve to remove water vapor from the chamber 1 during normal operation of the freeze-drying system.
  • the condensation surfaces usually consist of coils through which the refrigerant (for example chlorofluorocarbons) flows. The outer surfaces of these coils form the actual condensation surfaces.
  • the compressor refrigeration machine 5 also serves to supply the condensation surfaces 18 with refrigerant.
  • the condensation surfaces 18 can be connected to the refrigerant circuit 6 via the lines 19 and 21 with the valve 22.
  • the condenser 12 there is a further condensation surface 23, which is connected via the line 24 to the valve 25 to the lower region of a storage container 26.
  • the storage container 26 contains a low-boiling refrigerant 27, for example liquid nitrogen.
  • the line 28 is connected to the lower region of the storage container 26, which opens into its upper region above the refrigerant level.
  • an evaporator 29 and a pressure control valve 31 are switched on. With the aid of these elements, a certain pressure, for example a few bar, preferably 3 bar, can be maintained within the storage container 36.
  • An alternative, in which the further condensation surface is located inside the chamber 1, is shown in dashed lines.
  • the line 24 ⁇ connected to the reservoir 26 via the valve 25 opens into the condensation surface 23 ⁇ which is arranged next to the adjusting plates 2.
  • the freeze-drying device shown works as follows: after a sterilization process, the product is introduced into the chamber 1 and frozen. For this purpose, the temperature control medium flowing in the temperature control circuit 3 is brought to correspondingly low temperatures with the aid of the compressor refrigerator 5. The valve 15 is closed during the freezing phase.
  • valves 15 and 17 are opened and the temperature control medium flowing in the temperature control circuit 3 is warmed up.
  • the valve 9 in the refrigerant circuit 6 is closed and the heating, not shown, is put into operation.
  • the chamber 1 is evacuated to a pressure of about 10 ⁇ 1 mbar.
  • the condensation surfaces 18 serve to remove the relatively large amounts of water vapor during normal operation, which are cooled with the aid of the compressor refrigerator 5. Small amounts of permanent gases still present flow through the condenser 12 and are removed using the gas ballast pump 13.
  • the cooling for the condensation surfaces 18 fails.
  • the pumping speed for water vapor decreases and returns to 0 relatively quickly.
  • the water vapor escaping from the product is no longer removed. Since the temperature control medium in the temperature control circuit 3 is warm during the main and post-drying (room temperature or slightly above), the product on the setting plates 2 begins to heat up immediately. If the product thaws or thaws, there is often a loss of quality or even a change that renders the product unusable.
  • the condensation surface 23 is provided in the condenser 12.
  • the low-boiling refrigerant 27 enters the tube coil forming the condensation surface 23 from below, evaporates there and thus cools the condensation surface 23 very quickly to relatively low temperatures.
  • the evaporated refrigerant is discharged into the atmosphere via line 32, for example.
  • the condensation surface 23 takes effect before the water vapor absorbency of the condensation surfaces 18 has significantly decreased. The water vapor suction capacity of the condenser 12 is thus retained regardless of the operating medium, and that until the refrigerant is finally consumed in the storage container 26.
  • the emergency cooling can therefore be maintained for a sufficiently long time in order to be able to remedy the incident that has occurred.
  • valve 15 In the event of a malfunction, the valve 15 must keep its open position, close the valve 17 and open the valve 25.
  • These valves are therefore expediently equipped with electrical or electropneumatic actuating devices which are designed such that the valves 15 and 25 assume their open position in the event of a power failure and the valve 17 in its closed position in the event of a power failure. This ensures a safe function of the emergency cooling device.
  • valve 25 also opens in the event of a fault, while valve 15 closes.
  • the refrigerant 27 flows via line 24 ⁇ into the condensation surface 23 ⁇ , evaporates there and is discharged into the atmosphere via line 32 ⁇ .
  • the condensation surface 23 ⁇ becomes sufficiently cold to maintain the vacuum in the chamber 1. The product batch contained therein is therefore not endangered.

Abstract

The invention relates to a freeze-drying apparatus having a chamber (1) which can be evacuated and an evacuation system (11); this apparatus is fitted with an additional condensation surface (23, 23') which is connected via a valve (25) to a reservoir (26) containing a cooling agent (27) with a low boiling point; if, as a consequence of a failure, the pump power of the evacuation system fails, the valve (25) is opened so that the additional condensation surface takes over the pumping effect. <IMAGE>

Description

Die vorliegende Erfindung bezieht sich auf eine Einrichtung zur Gefriertrocknung mit einer evakuierbaren Kammer und einem Evakuierungssystem.The present invention relates to a device for freeze drying with an evacuable chamber and an evacuation system.

Die Gefriertrocknung wird in erster Linie zur Konservierung temperaturempfindlicher Produkte eingesetzt, deren Eigen­schaften erhalten bleiben sollen. In den bereichen Pharmazie, Biologie und Medizin findet die Gefriertrocknung ihr Haupt­anwendungsgebiet.Freeze drying is primarily used to preserve temperature-sensitive products, the properties of which should be retained. Freeze-drying is mainly used in the fields of pharmacy, biology and medicine.

Der übliche Gefriertrocknungsprozeß läuft etwa folgendermaßen ab: Nach dem Einfrieren des Wasser enthaltenden Produktes findet die Sublimation des in Eisform vorliegenden Wassers statt, und zwar unter vakuum (etwa 10⁻¹ mbar). Nach dieser Haupttrocknung findet die Nachtrocknung statt, während der die adsorptiv gebundene Feuchtigkeit entfernt wird, um extrem niedrige Restfeuchten zu erzielen. Während der Nach­trocknung wird das Produkt unter Einhaltung zulässiger Temperaturgrenzen erwärmt. Der Druck, bei dem die Nach­trocknung stattfindet, liegt bei etwa 10⁻³ mbar.The usual freeze-drying process takes place approximately as follows: after freezing the product containing water, the sublimation of the water in ice form takes place under vacuum (about 10uum¹ mbar). After this main drying, the post-drying takes place, during which the adsorptively bound moisture is removed in order to achieve extremely low residual moisture. During the final drying, the product is warmed up in compliance with permissible temperature limits. The pressure at which post-drying takes place is around 10⁻³ mbar.

Da die Gefriertrocknung im Chargenbetrieb durchgeführt wird, ist man bemüht, die Chargen möglichst groß zu wählen. Ent­sprechend hoch ist dann auch der Wert der Chargen. Es ist inzwischen durchaus üblich, mit Chargen zu fahren, deren Wert über 100 TDM liegt. Der Verlust der Charge infolge eines Störfalles führt deshalb zu empfindlichen Verlusten.Since freeze drying is carried out in batch operation, efforts are made to choose the batches as large as possible. The value of the batches is correspondingly high. It is now quite common to use batches with a value of more than 100 TDM. The loss of the batch as a result of an accident therefore leads to sensitive losses.

Folgende, eine Produktcharge gefährdende Störfälle können eintreten:
- Ausfall der Verdichter-Kältemaschinen, die die Produkt­stellflächen in der Vakuumkammer und die Kondensations­flächen im Kondensator mit Kühlmittel versorgen; dabei kann der Kältemittelverdichter selbst defekt gehen oder ein Verlust des Kältemittels aus dem Kältekreislauf eintreten;
- Stromausfall, komplett oder teilweise;
- Ausfall der Kühlung der Verflüssiger im Kühlmittelkreis­lauf der Kältemittelverdichter, wenn zum Beispiel die Wasserversorgung ausfällt;
- Ausfall der Anlagensteuerung.The following accidents that endanger a product batch can occur:
- Failure of the compressor chillers, which supply the product shelves in the vacuum chamber and the condensation surfaces in the condenser with coolant; the refrigerant compressor itself may fail or the refrigerant may be lost from the refrigeration cycle;
- power failure, complete or partial;
- Failure of the cooling of the condensers in the coolant circuit of the refrigerant compressors if, for example, the water supply fails;
- Failure of the system control.

Sämtliche dieser angegebenen Störfälle haben einen Ausfall der Kondensatorkühlung und damit einen Ausfall der Pump­leistung des Evakuierungssystems zur Folge. Da dem zu trocknenden Produkt während der Trocknung die für die Sublimation des Wassers erforderliche Energie in Form von Wärme zugeführt werden muß, führt ein Ausfall des Evaku­ierungssystems zu einer Erwärmung des Produktes, da vom Produkt abgegebener Wasserdampf nicht mehr abgepumpt wird. Gleichzeitig mit einem Druckanstieg in der Gefriertrock­nungskammer beginnt das Produkt aufzutauen. Dieser Vorgang führt insbesondere bei hochempfindlichen Medikamenten zu Qualitätsverlusten, unter Umständen zum Verlust der kom­pletten Gefriertrocknungscharge.All of these specified incidents result in a failure of the condenser cooling and thus a failure of the pumping capacity of the evacuation system. Since the product to be dried has to be supplied with the energy required for the sublimation of the water in the form of heat during the drying process, a failure of the evacuation system leads to heating of the product, since water vapor released by the product is no longer pumped out. At the same time as the pressure in the freeze drying chamber increases, the product begins to thaw. This process leads to a loss of quality, especially in the case of highly sensitive medications, and possibly to the loss of the entire freeze-drying batch.

Der vorliegenden Erfindung liegt die Aufgabe zugrunde, eine Gefriertrocknungseinrichtung der eingangs genannten Art zu schaffen, bei der die Produktchargen nicht mehr durch Störfälle der beschriebenen oder einer ähnlichen Art gefährdet sind.The present invention has for its object to provide a freeze-drying device of the type mentioned, in which the product batches are no longer at risk from accidents of the type described or a similar type.

Erfindungsgemäß wird diese Aufgabe dadurch gelöst, daß die Einrichtung zusätzlich mit einer Kondensationsfläche ausgerüstet ist, die über ein Ventil an einen Vorratsbehälter mit einem niedrigsiedenden Kältemittel angeschlossen ist. Bei einem Störfall wird das Ventil zwischen der weiteren Kondensationsfläche im Kondensator und dem Vorratsbehälter geöffnet, so daß das Kältemittel in die Kondensationsfläche einströmt. Die weitere Konden­sationsfläche übernimmt damit die Pumpwirkung. Das Vakuum in der Gefriertrocknungskammer bleibt betriebsmittelunabhängig erhalten, so daß die Gefahr des An- oder Auftauens des Produktes nicht besteht. Die zusätzliche Kondensationsfläche kann in der Gefriertrocknungskammer, in dem üblicherweise an die Gefriertrocknungskammer angeschlossenen Kondensator oder auch in einer separaten Kammer untergebracht sein.According to the invention, this object is achieved in that the device is additionally equipped with a condensation surface which is connected to a valve Storage container with a low-boiling refrigerant is connected. In the event of a malfunction, the valve between the further condensation surface in the condenser and the storage container is opened so that the refrigerant flows into the condensation surface. The further condensation surface thus takes over the pumping effect. The vacuum in the freeze-drying chamber remains independent of the equipment, so that there is no risk of thawing or thawing of the product. The additional condensation surface can be accommodated in the freeze-drying chamber, in the condenser that is usually connected to the freeze-drying chamber, or in a separate chamber.

Weitere Vorteile und Einzelheiten der Erfindung sollen anhand eines in der Figur schematisch dargestellten Aus­führungsbeispieles erläutert werden.Further advantages and details of the invention will be explained with reference to an exemplary embodiment shown schematically in the figure.

Die in der Figur dargestellte Einrichtung zur Gefriertrock­nung umfaßt die Vakuumkammer 1 mit den Stellflächen 2, auf denen sich das Produkt während des Ablaufs des Gefrier­trocknungsprozesses befindet. Üblicherweise sind die Stellflächen 2 sowohl kühlbar als auch aufheizbar. Dazu sind die Stellflächen 2 mit im einzelnen nicht dargestellten Hohlräumen ausgerüstet, die von einem Temperiermittel (zum Beispiel Silikonöl) durchströmt werden. Der Temperier­kreislauf ist strichpunktiert eingezeichnet und mit 3 bezeichnet. In diesen Temperaturkreislauf 3 sind die Stellplatten 2 parallel zueinander und die Förderpumpe 4 eingeschaltet. Soll das umströmende Kältemittel gekühlt werden, dann wird die Verdichter-Kältemaschine 5 in Betrieb gesetzt. Die Verdichter-Kältemaschine 5 befindet sich im Kältemittelkreislauf 6, der üblicherweise den mit Wasser gekühlten Verflüssiger 7, den Wärmetauscher 8 und das Ventil 9 umfaßt. Der Verflüssiger 7 ist vorzugsweise wassergekühlt. Der Wärmetauscher 8 ist in den Temperierkreislauf 3 eingeschaltet. Häufig werden mehrere Verdichter-Kältemaschinen an dieser Stelle eingesetzt, um entweder den Betrieb zu sichern (getrennte Kreisläufe) oder tiefere Temperaturen zu erreichen (Kaskadenschaltung). Auch der Einsatz einer anderen Kältemaschine (zum Beispiel Adsorptionskältemaschine) ist möglich.The device for freeze drying shown in the figure comprises the vacuum chamber 1 with the shelves 2 on which the product is located during the course of the freeze drying process. The shelves 2 are usually both coolable and heatable. For this purpose, the shelves 2 are equipped with cavities, not shown in detail, through which a temperature control agent (for example silicone oil) flows. The temperature control circuit is shown in dash-dot lines and labeled 3. In this temperature circuit 3, the setting plates 2 are parallel to each other and the feed pump 4 is switched on. If the circulating refrigerant is to be cooled, then the compressor refrigeration machine 5 is started up. The compressor refrigeration machine 5 is located in the refrigerant circuit 6, which usually comprises the water-cooled condenser 7, the heat exchanger 8 and the valve 9. The condenser 7 is preferably water-cooled. The heat exchanger 8 is in the Temperature control circuit 3 switched on. Often, several compressor chillers are used at this point in order to either ensure operation (separate circuits) or to reach lower temperatures (cascade connection). Another chiller (e.g. adsorption chiller) can also be used.

Die Erwärmung der Stellplatten 2 erfolgt üblicherweise mittels einer im einzelnen nicht dargestellten elektrischen Beheizung des im Temperierkreislauf 3 umlaufenden Temperiermittels. Auch die Verwendung der Abwärme der Kältemaschinen oder der Einsatz dampfbeheizter Wärmetauscher ist möglich.The heating of the setting plates 2 is usually carried out by means of an electrical heating, not shown in detail, of the temperature control medium circulating in the temperature control circuit 3. The use of waste heat from the chillers or the use of steam-heated heat exchangers is also possible.

An die Vakuumkammer 1 ist ein Evakuierungssystem 11 ange­schlossen, das einen Kondensator 12 und eine Vakuumpumpe 13 (Gasballastpumpe) umfaßt. In der Verbindungsleitung 14 zwischen Vakuumkammer 1 und Kondensator 12 befindet sich das Ventil 15. Zwischen Kondensator 12 und Vakuumpumpe 13 erstreckt sich die Leitung 16 mit dem Ventil 17.An evacuation system 11 is connected to the vacuum chamber 1 and comprises a condenser 12 and a vacuum pump 13 (gas ballast pump). The valve 15 is located in the connecting line 14 between the vacuum chamber 1 and the condenser 12. The line 16 with the valve 17 extends between the condenser 12 and the vacuum pump 13.

Innerhalb des Kondensators 12 sind eine oder mehrere Konden­sationsflächen 18 untergebracht, die während des Normal­betriebs der Gefriertrocknungsanlage der Entfernung von Wasserdampf aus der Kammer 1 dienen. Die Kondensations­flächen bestehen üblicherweise aus Rohrschlangen, die von dem Kältemittel (zum Beispiel Fluorchlorkohlenwasserstoffe) durchströmt sind. Die Außenflächen dieser Rohrschlangen bilden die eigentlichen Kondensationsflächen. Der Versor­gung der Kondensationsflächen 18 mit Kältemittel dient ebenfalls die Verdichterkältemaschine 5. Über die Leitungen 19 und 21 mit dem Ventil 22 sind die Kondensa­tionsflächen 18 an den Kältemittelkreislauf 6 anschließbar.One or more condensation surfaces 18 are accommodated within the condenser 12 and serve to remove water vapor from the chamber 1 during normal operation of the freeze-drying system. The condensation surfaces usually consist of coils through which the refrigerant (for example chlorofluorocarbons) flows. The outer surfaces of these coils form the actual condensation surfaces. The compressor refrigeration machine 5 also serves to supply the condensation surfaces 18 with refrigerant. The condensation surfaces 18 can be connected to the refrigerant circuit 6 via the lines 19 and 21 with the valve 22.

Im Kondensator 12 befindet sich eine weitere Kondensations­fläche 23, die über die Leitung 24 mit dem Ventil 25 an den unteren Bereich eines Vorratsbehälters 26 angeschlossen ist. Der Vorratsbehälter 26 enthält ein niedrigsiedendes Kältemittel 27, beispielsweise flüssigen Stickstoff. Weiterhin ist an den unteren Bereich des Vorratsbehälters 26 die Leitung 28 angeschlossen, die in seinen oberen Bereich oberhalb des Kältemittelspiegels mündet. In dieser Leitung sind ein Verdampfer 29 und ein Druckregelventil 31 einge­schaltet. Mit Hilfe dieser Elemente kann innerhalb des Vorratsbehälters 36 ein bestimmter Druck, beispielsweise einige Bar, vorzugsweise 3 bar, aufrechterhalten werden. Eine Alternative, bei der sich die weitere Kondensations­fläche innerhalb der Kammer 1 befindet, ist gestrichelt dargestellt. Die über das Ventil 25 mit dem Vorrats­behälter 26 verbundene Leitung 24ʹ mündet in die Kondensa­tionsfläche 23ʹ, die neben den Stellplatten 2 angeordnet ist.In the condenser 12 there is a further condensation surface 23, which is connected via the line 24 to the valve 25 to the lower region of a storage container 26. The storage container 26 contains a low-boiling refrigerant 27, for example liquid nitrogen. Furthermore, the line 28 is connected to the lower region of the storage container 26, which opens into its upper region above the refrigerant level. In this line, an evaporator 29 and a pressure control valve 31 are switched on. With the aid of these elements, a certain pressure, for example a few bar, preferably 3 bar, can be maintained within the storage container 36. An alternative, in which the further condensation surface is located inside the chamber 1, is shown in dashed lines. The line 24ʹ connected to the reservoir 26 via the valve 25 opens into the condensation surface 23ʹ which is arranged next to the adjusting plates 2.

Die dargestellte Gefriertrocknungseinrichtung arbeitet folgendermaßen: Nach einem Sterilisationsvorgang wird das Produkt in die Kammer 1 eingebracht und eingefroren. Dazu wird das im Temperierkreislauf 3 strömende Temperiermittel mit Hilfe der Verdichter-Kältemaschine 5 auf entsprechend niedrige Temperaturen gebracht. Das Ventil 15 ist während der Einfrierphase geschlossen.The freeze-drying device shown works as follows: after a sterilization process, the product is introduced into the chamber 1 and frozen. For this purpose, the temperature control medium flowing in the temperature control circuit 3 is brought to correspondingly low temperatures with the aid of the compressor refrigerator 5. The valve 15 is closed during the freezing phase.

Zur Durchführung der Haupttrocknung werden die Ventile 15 und 17 geöffnet und das im Temperierkreislauf 3 strömende Temperiermittel aufgewärmt. Dazu wird das Ventil 9 im Kältemittelkreislauf 6 geschlossen und die nicht darge­stellte Beheizung in Betrieb gesetzt.To carry out the main drying, the valves 15 and 17 are opened and the temperature control medium flowing in the temperature control circuit 3 is warmed up. For this purpose, the valve 9 in the refrigerant circuit 6 is closed and the heating, not shown, is put into operation.

Die Kammer 1 wird auf einen Druck von etwa 10⁻¹ mbar evakuiert. Der Entfernung der relativ großen Wasserdampf­mengen dienen bei Normalbetrieb die Kondensationsflächen 18, die mit Hilfe der Verdichter-Kältemaschine 5 gekühlt werden. Geringe Mengen noch vorhandener Permanentgase durch­strömen den Kondensator 12 und werden mit Hilfe der Gas­ballastpumpe 13 entfernt.The chamber 1 is evacuated to a pressure of about 10⁻¹ mbar. The condensation surfaces 18 serve to remove the relatively large amounts of water vapor during normal operation, which are cooled with the aid of the compressor refrigerator 5. Small amounts of permanent gases still present flow through the condenser 12 and are removed using the gas ballast pump 13.

Tritt einer der eingangs beschriebenen Störfälle ein, dann fällt die Kühlung für die Kondensationsflächen 18 aus. Das Saugvermögen für Wasserdampf nimmt ab und geht relativ schnell auf 0 zurück. Der aus dem Produkt entweichende Wasserdampf wird nicht mehr abgeführt. Da das Temperier­mittel im Temperierkreislauf 3 während der Haupt- und der Nachtrocknung warm ist (Zimmertemperatur oder etwas darüber), beginnt sofort eine Erwärmung des auf den Stell­platten 2 befindlichen Produktes. Taut das Produkt an oder auf, tritt häufig ein Qualitätsverlust oder gar eine Veränderung ein, durch die das Produkt unbrauchbar wird.If one of the malfunctions described at the outset occurs, then the cooling for the condensation surfaces 18 fails. The pumping speed for water vapor decreases and returns to 0 relatively quickly. The water vapor escaping from the product is no longer removed. Since the temperature control medium in the temperature control circuit 3 is warm during the main and post-drying (room temperature or slightly above), the product on the setting plates 2 begins to heat up immediately. If the product thaws or thaws, there is often a loss of quality or even a change that renders the product unusable.

Um bei einem Störfall dieser Art das Wasserpumpsaugvermögen des Kondensators 12 betriebsmittelunabhängig, das heißt, unabhängig von den beim Normalbetrieb der Gefriertrocknungs­anlage erforderlichen Mittel wie Strom, Wasser und der­gleichen, aufrechterhalten zu können, ist im Kondensator 12 die Kondensationsfläche 23 vorgesehen. Durch Öffnen des Ventils 25 gelangt das niedrigsiedende Kältemittel 27 von unten in die die Kondensationsfläche 23 bildende Rohr­schlange, verdampft dort und kühlt damit die Kondensations­fläche 23 sehr schnell auf relativ tiefe Temperaturen ab. Das verdampfte Kältemittel wird über die Leitung 32 zum Beispiel in die Atmosphäre abgeführt. Die Kondensations­fläche 23 wird wirksam, bevor das Wasserdampfsaugvermögen der Kondensationsflächen 18 maßgeblich abgenommen hat. Das Wasserdampfsaugvermögen des Kondensators 12 bleibt damit betriebsmittelunabhängig erhalten, und zwar bis zum end­gültigen Verbrauch des Kältemittels im Vorratsbehälter 26.In order to be able to maintain the water pumping capacity of the condenser 12 independently of the operating medium in the event of a malfunction of this type, that is to say independently of the means such as electricity, water and the like required during normal operation of the freeze drying system, the condensation surface 23 is provided in the condenser 12. By opening the valve 25, the low-boiling refrigerant 27 enters the tube coil forming the condensation surface 23 from below, evaporates there and thus cools the condensation surface 23 very quickly to relatively low temperatures. The evaporated refrigerant is discharged into the atmosphere via line 32, for example. The condensation surface 23 takes effect before the water vapor absorbency of the condensation surfaces 18 has significantly decreased. The water vapor suction capacity of the condenser 12 is thus retained regardless of the operating medium, and that until the refrigerant is finally consumed in the storage container 26.

Bei einer entsprechenden Wahl der Größe des Vorrats an Kältemittel 27 kann deshalb die Notkühlung ausreichend lange aufrechterhalten werden, um den eingetretenen Störfall beheben zu können.With a corresponding choice of the size of the supply of refrigerant 27, the emergency cooling can therefore be maintained for a sufficiently long time in order to be able to remedy the incident that has occurred.

Bei Eintritt eines Störfalles muß das Ventil 15 seine offene Stellung behalten, das Ventil 17 schließen und das Ventil 25 öffnen. Zweckmäßigerweise sind diese Ventile deshalb mit elektrischen oder elektropneumatischen Betätigungseinrichtungen ausgerüstet, die derart ausge­bildet sind, daß die Ventile 15 und 25 bei Stromausfall ihre Offenstellung und das Ventil 17 bei Stromausfall seine Schließstellung einnehmen. Eine sichere Funktion der Notkühleinrichtung wird dadurch erreicht.In the event of a malfunction, the valve 15 must keep its open position, close the valve 17 and open the valve 25. These valves are therefore expediently equipped with electrical or electropneumatic actuating devices which are designed such that the valves 15 and 25 assume their open position in the event of a power failure and the valve 17 in its closed position in the event of a power failure. This ensures a safe function of the emergency cooling device.

Bei der gestrichelt dargestellten Alternativlösung öffnet sich ebenfalls im Störfall das Ventil 25, während das Ventil 15 schließt. Das Kältemittel 27 strömt über die Leitung 24ʹ in die Kondensationsfläche 23ʹ, verdampft dort und wird über die Leitung 32ʹ in die Atmosphäre abgeführt. Unmittelbar nach dem Eintritt des Störfalles wird die Kondensationsfläche 23ʹ ausreichend kalt, um das Vakuum in der Kammer 1 aufrechtzuerahalten. Die darin befindliche Produktcharge ist somit nicht gefährdet.In the alternative solution shown in dashed lines, valve 25 also opens in the event of a fault, while valve 15 closes. The refrigerant 27 flows via line 24ʹ into the condensation surface 23ʹ, evaporates there and is discharged into the atmosphere via line 32ʹ. Immediately after the occurrence of the accident, the condensation surface 23ʹ becomes sufficiently cold to maintain the vacuum in the chamber 1. The product batch contained therein is therefore not endangered.

Claims (10)

1. Einrichtung zur Gefriertrocknung mit einer evakuierbaren Kammer (1) und einem Evakuierungssystem (11), dadurch gekennzeichnet, daß die Einrichtung zusätzlich mit einer Kondensationsfläche (23, 23ʹ) ausgerüstet ist, die über ein Ventil (25) an einen Vorratsbehälter (26) mit einem niedrigsiedenden Kältemittel (27) angeschlossen ist.1. Device for freeze-drying with an evacuable chamber (1) and an evacuation system (11), characterized in that the device is additionally equipped with a condensation surface (23, 23ʹ) which is connected to a storage container (26) via a valve (25). with a low-boiling refrigerant (27) is connected. 2. Einrichtung nach Anspruch 1, dadurch gekennzeichnet, daß das Evakuierungssystem (11) einen Kondensator (12) mit mindestens einer von einer Kältemaschine (5) versorgten Kondensationsfläche (18) umfaßt und daß sich die weitere Kondensationsfläche (23) im Kondensator (12) befindet.2. Device according to claim 1, characterized in that the evacuation system (11) comprises a condenser (12) with at least one condensation surface (18) supplied by a refrigerator (5) and in that the further condensation surface (23) in the condenser (12) located. 3. Einrichtung nach Anspruch 1, dadurch gekennzeichnet, daß sich die weitere Kondensationsfläche (23ʹ) in der Kammer (1) befindet.3. Device according to claim 1, characterized in that the further condensation surface (23ʹ) is in the chamber (1). 4. Einrichtung nach einem der Ansprüche 1 bis 3, dadurch gekennzeichnet, daß das Evakuierungssystem (11) aus dem Kondensator (12) und einer Vakuumpumpe (13) besteht, die über die Leitung (16) mit dem Ventil (17) verbunden sind.4. Device according to one of claims 1 to 3, characterized in that the evacuation system (11) consists of the condenser (12) and a vacuum pump (13) which are connected via the line (16) to the valve (17). 5. Einrichtung nach einem der Ansprüche 1 bis 4, dadurch gekennzeichnet, daß sich zwischen der evakuier­baren Kammer (1) und dem Kondensator (12) eine Leitung (14) mit einem Ventil (15) befindet.5. Device according to one of claims 1 to 4, characterized in that there is a line (14) with a valve (15) between the evacuable chamber (1) and the capacitor (12). 6. Einrichtung nach Anspruch 2, 4 und 5, dadurch gekenn­zeichnet, daß die Ventile (15, 17 und 25) mit elektri­schen oder elektropneumatischen Betätigungseinrich­tungen ausgerüstet sind, derart, daß bei Stromausfall das Ventil (17) seine Schließstellung und die Ventile (15 und 25) ihre Offenstellung einnehmen beziehungsweise beibehalten.6. Device according to claim 2, 4 and 5, characterized in that the valves (15, 17 and 25) are equipped with electrical or electropneumatic actuators, such that the valve (17) its closed position and the valves (15 and 25) assume or maintain their open position. 7. Einrichtung nach Anspruch 3, 4 und 5, dadurch gekenn­zeichnet, daß die Ventile (15 und 25) mit elektri­schen oder elektropneumatischen Betätigungseinrich­tungen ausgerüstet sind, derart, daß bei Stromausfall das Ventil (15) seine Schließstellung und das Ventil (25) seine Offenstellung einnehmen.7. Device according to claim 3, 4 and 5, characterized in that the valves (15 and 25) are equipped with electrical or electropneumatic actuators, such that the valve (15) its closed position and the valve (25) its in the event of a power failure Take open position. 8. Einrichtung nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, daß dem Vorratsbehälter (26) für das flüssige Kältemittel (27) Mittel (28,29,31) zugeordnet sind, die der Erzeugung eines erhöhten Behälterinnendruckes dienen.8. Device according to one of the preceding claims, characterized in that the reservoir (26) for the liquid refrigerant (27) are assigned means (28, 29, 31) which serve to generate an increased internal pressure in the container. 9. Einrichtung nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, daß das Kältemittel (27) im Vorratsbehälter (26) flüssiger Stickstoff ist.9. Device according to one of the preceding claims, characterized in that the refrigerant (27) in the reservoir (26) is liquid nitrogen. 10. Verfahren zum Betrieb einer Einrichtung nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, daß bei einem Störfall die Kondensationsfläche (23,23ʹ) mit dem niedrigsiedenden Kältemittel (27) gekühlt wird.10. A method of operating a device according to one of the preceding claims, characterized in that the condensation surface (23, 23ʹ) is cooled with the low-boiling refrigerant (27) in the event of a malfunction.
EP87110955A 1987-07-29 1987-07-29 Freeze-drying apparatus Expired - Lifetime EP0301117B1 (en)

Priority Applications (5)

Application Number Priority Date Filing Date Title
EP87110955A EP0301117B1 (en) 1987-07-29 1987-07-29 Freeze-drying apparatus
DE3750847T DE3750847D1 (en) 1987-07-29 1987-07-29 Freeze-drying facility.
ES87110955T ES2068809T3 (en) 1987-07-29 1987-07-29 DEVICE FOR LYOPHILIZATION.
JP63173852A JP2676374B2 (en) 1987-07-29 1988-07-14 Freeze dryer
US07/226,536 US4949473A (en) 1987-07-29 1988-07-29 Freeze drying apparatus with additional condensation surface and refrigeration source

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
EP87110955A EP0301117B1 (en) 1987-07-29 1987-07-29 Freeze-drying apparatus

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EP0301117A1 true EP0301117A1 (en) 1989-02-01
EP0301117B1 EP0301117B1 (en) 1994-12-07

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EP87110955A Expired - Lifetime EP0301117B1 (en) 1987-07-29 1987-07-29 Freeze-drying apparatus

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US (1) US4949473A (en)
EP (1) EP0301117B1 (en)
JP (1) JP2676374B2 (en)
DE (1) DE3750847D1 (en)
ES (1) ES2068809T3 (en)

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DE4233479A1 (en) * 1991-10-04 1993-05-13 Inst Mikrobiologie Und Biochem Microorganism freeze drying - using double-walled condenser with constant selected temps. in each drying phase
EP0651212A2 (en) * 1993-11-01 1995-05-03 The Boc Group, Inc. Heat exchange systems
EP0989376A3 (en) * 1998-09-21 2000-04-12 Praxair Technology, Inc. Freeze drying with reduced cryogen consumption
CN105452791A (en) * 2013-05-29 2016-03-30 基伊埃工程技术股份有限公司 Method of providing inline sterile freeze drying of a product in trays accommodated in a trolley, system for carrying out the method, and use of the method
EP3338810A1 (en) * 2016-12-05 2018-06-27 Innovations-Transfer Uphoff GmbH & Co. KG Method and device for drying in steam explosion method
CN111504003A (en) * 2020-03-30 2020-08-07 广西农业职业技术学院 Freeze drying method and drying device thereof

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US5199187A (en) * 1991-07-31 1993-04-06 Sp Industries Freeze dryer apparatus having an interim condensing system and use thereof
JPH0735951B2 (en) * 1991-10-30 1995-04-19 西部瓦斯株式会社 Vacuum drying treatment device
US5291751A (en) * 1992-04-21 1994-03-08 Liquid Carbonic Corporation Cryo-mechanical vapor recovery apparatus
US6122836A (en) * 1998-05-07 2000-09-26 S.P. Industries, Inc., The Virtis Division Freeze drying apparatus and method employing vapor flow monitoring and/or vacuum pressure control
WO2000040910A1 (en) * 1999-01-05 2000-07-13 Universal Preservation Technologies, Inc. Vacuum control system for foam drying apparatus
WO2005073652A2 (en) * 2004-02-02 2005-08-11 I.M.T. Interface Multigrad Technology Ltd. Apparatus, system and method for lyophilization
WO2011071676A1 (en) 2009-12-11 2011-06-16 Wyssmont Company Inc. Apparatus and method for continuous lyophilization
US9194626B2 (en) * 2009-12-22 2015-11-24 Ima Life North America Inc. Monitoring freeze drying with gas measurement on vacuum pump exhaust
CN103123206A (en) * 2013-03-21 2013-05-29 楚天科技股份有限公司 Freeze dryer
CN103344096A (en) * 2013-07-18 2013-10-09 上海千山远东制药机械有限公司 Freeze dryer water catcher
CN105509422B (en) * 2015-12-24 2018-09-25 甘肃银光化学工业集团有限公司 A kind of vacuum freeze-drying system and using the system to the method for energetic material vacuum freeze drying
CN106468501B (en) * 2016-08-29 2019-12-27 浙江金石生物科技有限公司 Nitrogen-protected dendrobium officinale freeze-drying device and freeze-drying method thereof
CN108469151B (en) * 2018-02-10 2023-04-14 扬子江药业集团南京海陵药业有限公司 Freeze-drying process for commercial production of disodium levoornidazole phosphate for injection
WO2020201822A2 (en) * 2019-01-27 2020-10-08 Nguyen Vien Lam Convection current freeze drying apparatus and method of operating the same
CN113865273B (en) * 2021-09-01 2023-01-31 广州韩秀科技有限公司 Open negative pressure low-temperature drying equipment

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FR2665338A1 (en) * 1990-08-02 1992-02-07 Blaizat Claude Method of concentrating and dehydrating a beverage (food liquid) or the like, relevant device and the product obtained
EP0499006A1 (en) * 1990-08-02 1992-08-19 Claude Blaizat Concentrating, dehydrating process for alimentory liquid or the same, apparatus therefor and product so made
DE4233479A1 (en) * 1991-10-04 1993-05-13 Inst Mikrobiologie Und Biochem Microorganism freeze drying - using double-walled condenser with constant selected temps. in each drying phase
DE4233479C2 (en) * 1991-10-04 1999-09-02 Inst Mikrobiologie Und Biochem Method and device for freeze drying, in particular liquids with microorganisms
EP0651212A2 (en) * 1993-11-01 1995-05-03 The Boc Group, Inc. Heat exchange systems
EP0651212A3 (en) * 1993-11-01 1997-10-08 Boc Group Inc Heat exchange systems.
EP0989376A3 (en) * 1998-09-21 2000-04-12 Praxair Technology, Inc. Freeze drying with reduced cryogen consumption
CN105452791A (en) * 2013-05-29 2016-03-30 基伊埃工程技术股份有限公司 Method of providing inline sterile freeze drying of a product in trays accommodated in a trolley, system for carrying out the method, and use of the method
CN105452791B (en) * 2013-05-29 2017-05-31 基伊埃工程技术股份有限公司 Inline sterilizing freeze-drying is provided and is contained in the method for product in handcart pallet, the system for performing the method and the use to the method
US9863700B2 (en) 2013-05-29 2018-01-09 Gea Process Engineering A/S Method of providing inline sterile freeze drying of a product in trays accommodated in a trolley, system for carrying out the method, and use of the method
EP3338810A1 (en) * 2016-12-05 2018-06-27 Innovations-Transfer Uphoff GmbH & Co. KG Method and device for drying in steam explosion method
CN111504003A (en) * 2020-03-30 2020-08-07 广西农业职业技术学院 Freeze drying method and drying device thereof

Also Published As

Publication number Publication date
US4949473A (en) 1990-08-21
JP2676374B2 (en) 1997-11-12
JPS6449882A (en) 1989-02-27
ES2068809T3 (en) 1995-05-01
DE3750847D1 (en) 1995-01-19
EP0301117B1 (en) 1994-12-07

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