WO1995010744A1 - Freeze-drying plant - Google Patents

Freeze-drying plant Download PDF

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Publication number
WO1995010744A1
WO1995010744A1 PCT/EP1994/002426 EP9402426W WO9510744A1 WO 1995010744 A1 WO1995010744 A1 WO 1995010744A1 EP 9402426 W EP9402426 W EP 9402426W WO 9510744 A1 WO9510744 A1 WO 9510744A1
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WO
WIPO (PCT)
Prior art keywords
drying
weighing
mass
freeze
drying chamber
Prior art date
Application number
PCT/EP1994/002426
Other languages
German (de)
French (fr)
Inventor
Martin Christ
Original Assignee
Martin Christ Gefriertrocknungsanlagen Gmbh
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Martin Christ Gefriertrocknungsanlagen Gmbh filed Critical Martin Christ Gefriertrocknungsanlagen Gmbh
Priority to DE59404209T priority Critical patent/DE59404209D1/en
Priority to EP94924796A priority patent/EP0672234B1/en
Publication of WO1995010744A1 publication Critical patent/WO1995010744A1/en

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Classifications

    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F26—DRYING
    • F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
    • F26B25/00—Details of general application not covered by group F26B21/00 or F26B23/00
    • F26B25/22—Controlling the drying process in dependence on liquid content of solid materials or objects
    • F26B25/225—Controlling the drying process in dependence on liquid content of solid materials or objects by repeated or continuous weighing of the material or a sample thereof
    • 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 invention relates to a freeze drying system according to the preamble of claim 1.
  • the freeze drying process can be optimized with a moisture determination, which can be achieved, for example, by weighing the mass of the drying substance.
  • a moisture determination which can be achieved, for example, by weighing the mass of the drying substance.
  • Different systems or process technologies are known for weighing, each of which has specific disadvantages.
  • Another measuring principle is that a sample of the drying substance by means of a vacuum lock
  • a weighing device according to which the mass of a vessel standing on a shelf with direct contact can be measured directly is hereby. This means that for the mass of all vessels in the entire system, including the mass to be weighed, the same thermal and other at all times
  • the weighing device is designed as an electrical weighing device which, on the output side, supplies an electrical measured value corresponding to the mass to be measured, which can be transferred in a suitable manner and processed in external measuring and evaluation systems. The latter transmission can take place via suitable measuring lines, which are laid through vacuum-tight bushings through the wall of the drying chamber. This eliminates dynamic seals.
  • Another important advantage of this system is that the measuring process can be repeated at short intervals in accordance with the dynamics of the electrical measuring principle, and in this way practically continuous mass determination and thus control of the course of each phase of the drying process is possible.
  • a measured value of the initial liquid mass including that of the vessel
  • the residual moisture can be determined taking into account the measured value of the dry mass and that of the vessel.
  • the further evaluation of this measured value which relates to the mass of the drying substance, can be carried out in any manner, that is, it can also be used to optimize the freeze-drying process.
  • the electrical measured value a wide variety of different thermal and other physical conditions of the measuring process can be taken into account, so that the measuring accuracy is ensured.
  • Gripper arm is connected to a vessel.
  • a vessel There is usually a large number of individual vessels on a shelf and there is the possibility of providing one or more weighing devices of this type, each of which is assigned to a shelf, so that, if necessary, several measurements can be carried out in relation to the vessels of a shelf. The measurement results can then be regarded as representative of the totality of all the vessels in a footprint.
  • a weighing device or a weighing cell can also be equipped with a plurality of gripping arms and can thus be determined and designed for the simultaneous or successive determination of the mass of a plurality of vessels.
  • the load cell can be arranged in a stationary manner in the drying chamber or in a secondary chamber connected to the drying chamber, so that, for the purpose of carrying out a measuring process, the positioning plate on which the respective vessel stands is lowered so that the vessel to be weighed is during the measuring process is held exclusively over the gripper arm.
  • the load cell can be arranged in a stationary manner in the drying chamber or in a secondary chamber connected to the drying chamber, so that, for the purpose of carrying out a measuring process, the positioning plate on which the respective vessel stands is lowered so that the vessel to be weighed is during the measuring process is held exclusively over the gripper arm.
  • the load cell can be arranged in a stationary manner in the drying chamber or in a secondary chamber connected to the drying chamber, so that, for the purpose of carrying out a measuring process, the positioning plate on which the respective vessel stands is lowered so that the vessel to be weighed is during the measuring process is held exclusively over the gripper arm.
  • the measuring process can be carried out briefly and thus quasi continuously, and that the drying substance is measured under conditions which correspond to those of the other vessels of a positioning plate, so that the measuring process is representative of the totality of the respective vessels at least one Stand plate can be viewed.
  • maximum quantities of a drying substance are dried and the sample to be measured remains usable.
  • the gripping arm of the load cell is expediently designed in such a way that every selectable position on a footprint can be reached, so that it is also ensured that representative measurement conditions can be maintained.
  • the principle according to the invention is not dependent on the fact that the drying substance is held in certain vessels - bowls, vials or other drying vessels can also be present to hold the drying substance.
  • the drawing shows a freeze-drying system which consists globally of a drying chamber 1 and a condenser chamber 2 which are connected to one another via a passage 3 which can be closed by means of a valve (not shown in the drawing).
  • chambers are arranged next to one another - however, they can equally well be arranged one above the other.
  • the capacitor can also be installed in the drying chamber.
  • the condenser chamber 2 is also connected via a line 7 to a vacuum generator 0.
  • the drying chamber contains, among other things, a system of stacking plates 9 arranged one above the other, which are inserted into a guide or displacement device (not shown in the drawing) and can be displaced in the direction of the arrows 10, thus perpendicular to their plane. The displacement takes place in such a way that the distance between all the setting plates 9 can be reduced in this way.
  • the displacement is triggered by a pressure plate 11 which is connected to a schematically illustrated drive 12 in a connection not shown in the drawing.
  • the drive 12 is located below the drying chamber. However, it can also be arranged above the drying chamber.
  • the drive 12 can be configured, for example, as a piston-cylinder unit to which pressure medium can be applied on both sides. However, this will not be discussed further below.
  • the setting plates 9 can be designed to be temperature-controlled in a manner known per se and serve as setting surfaces for vials 13, which are closed, for example, by means of vacuum plugs 14. These vials contain the drying substance, the stoppers mentioned having the property of allowing vapors to escape from the drying substance in the loosely attached state, but sealing the vial 13 in a vacuum-tight manner when pressed in.
  • the vials 13 are inserted with loosely placed vacuum plugs into the drying chamber 1, for example provided with a closable opening on the front.
  • the system of the setting plates 9 is moved in such a way that the plates move towards one another, so that in this way the vacuum plugs are pressed into the bottles 13 in order to close them in a vacuum-tight manner.
  • load cells 15 are arranged on or in the drying chamber 1, which are preferably based on an electrical measuring principle and are connected to a higher-level control, a PC or the like via measuring lines (not shown in the drawing).
  • Each of these load cells is connected to a vial 13 via a gripping arm 16, which is adapted to their respective arrangement inside or on the drying chamber 1, the direct connection of the gripping arm 16 to the vial 13 at its special geometry being shown in the drawing is not shown adapted.
  • the load cell 15 is located on the upper pressure plate 11 ', which is immovable relative to the walls of the drying chamber 1, the gripping arm 16 gripping a vial 13 on the positioning plate 9 located immediately below it.
  • a weighing process can be carried out in such a way that the setting plate 9 is lowered so that the vial hangs exclusively on the gripping arm 16.
  • the vial 13 can also be raised briefly via the load cell 15 with the position of the positioning plate 9 unchanged via the gripping arm 16.
  • the weighing cell 15 is located directly next to the vial 13 to be weighed on a positioning plate 9. In this case, the weighing operation can only be done by briefly lifting the vial 13 be effected.
  • the weighing cell 15 can also be accommodated in a stationary manner within the drying chamber 1, for example on a console, platform or the like, a weighing process in turn being able to be carried out in accordance with the two basic variants set out above.
  • the load cell 15 can also be arranged in a secondary chamber 17, which is connected to the drying chamber 1 via a connecting channel 18, the connecting channel 18 serving to receive the gripping arm 16.
  • the weighing process can be carried out according to the two principles already outlined above.
  • the weighing process can be carried out very quickly, without having to intervene in the drying process as a result of the measuring process.
  • this enables a repeatable measurement at any time, so that the drying process can be practically continuously monitored in this way, so that, for example, statements about the mass loss per unit of time - starting from the liquid to the completely dried state of the product - in the freeze drying phase are possible and also the influence of other process variables of the drying process, such as pressure and temperature, but also of other design parameters of the drying system, such as different flow cross sections of the passage 3 connecting the drying chamber 1 to the condenser chamber 2 or the position of the valve arranged here can be examined.
  • the residual moisture content in the product and the end of the freeze-drying process at a certain residual moisture can be determined.
  • the measurement result is expediently available in digitally coded form at the output of the load cells, so that it can be fed directly into an EDP system for further evaluation via appropriately designed interfaces.

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • General Engineering & Computer Science (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Molecular Biology (AREA)
  • Drying Of Solid Materials (AREA)

Abstract

A freeze-drying plant consisting overall of a condenser chamber (2) and a drying chamber (1), the drying chamber (1) of which is fitted with a system of superimposed, possibly adjustable supporting plates (9) acting as supports for phials (13) containing a drying substance, is fitted for the continuous determination of the mass of the drying substance and hence to monitor the drying cycle with weighing cells (15) connected to a phial (13) via a clamp arm (16). The weighing cells (15) are either permanently fitted inside the drying chamber (1), e.g. on its wall or on components which cannot move in relation to the wall, or they are directly on the supporting plates (9). The basis of the weighing principle of said weighing cells (15) is that either the supporting plate (9) of the phial (13) concerned is lowered with the weighing cell (15) in a constant position or the weighing cell (15) comprises a lifting device by means of which the phial (13) can be briefly raised. It is thus possible, together with fast measurement processes, to determine the mass of the drying substance virtually continuously without disturbing the drying process.

Description

B E S C H R E I B U N G DESCRIPTION
GefriertrocknungsanlageFreeze dryer
Die Erfindung bezieht sich auf eine Gefriertrocknungsan¬ lage entsprechend dem Oberbegriff des Anspruchs 1.The invention relates to a freeze drying system according to the preamble of claim 1.
Die Optimierung des Gefriertrocknungsprozesses kann mit einer Feuchtbestimmung erfolgen, welche beispielsweise durch Wiegen der Masse der Trocknungssubstanz erreichbar ist. Zum Wiegen sind unterschiedliche Systeme bzw. Verfahrenstechniken bekannt, denen jeweils spezifische Nachteile anhaften.The freeze drying process can be optimized with a moisture determination, which can be achieved, for example, by weighing the mass of the drying substance. Different systems or process technologies are known for weighing, each of which has specific disadvantages.
In diesem Zusammenhang sind z.B. Einrichtungen bekannt, bei denen sich die Trocknungssubstanz auf einem Wägetisch einer mechanischen oder einer elektrischen Wägeeiπrich- tung befindet. Nachdem die Trocknungssubstanz während des Trocknungsprozesses jedoch üblicherweise auf einer kühl- und/oder beheizbaren Stellfläche untergebracht ist, sind diese Messungen relativ ungenau und nicht repräsentativ, da die Trocknungssubstanz keinen direkten Kontakt mit den kühl- und/oder beheizbaren Stellflächen hat.In this context, e.g. Devices are known in which the drying substance is on a weighing table of a mechanical or an electrical weighing device. However, since the drying substance is usually housed on a coolable and / or heatable shelf during the drying process, these measurements are relatively imprecise and not representative, since the dry substance has no direct contact with the coolable and / or heatable shelves.
Ein weiteres Meßprinzip besteht darin, daß eine Probe der Trocknungssubstanz über eine Vakuumschleuse mittelsAnother measuring principle is that a sample of the drying substance by means of a vacuum lock
BERICHTIGTES BLATT (REGEL 81) ISA/EP eines Greif echanismus erfaßt und zwecks Bestimmung deren Masse während des Gefriertrocknungsprozesses der Trockπungska mer entnommen wird. Kontinuierliche Messun¬ gen oder zumindest angenähert kontinuierliche Messungen sind hierbei nicht möglich. Außerdem ist dieses System technisch unter anderem wegen der notwendigen Transport¬ vorgänge sehr aufwendig und darüber hinaus kosteninten¬ siv. Dies wird besonders deutlich, wenn ein, eine Trock¬ nungssubstanz enthaltendes Gefäß zwecks Probenentnahme nicht am Rand der Stellfläche sondern in deren Mitte aufgenommen werden soll, da ein entsprechend großer Abstand der Stellflächen erforderlich ist, um das, die Probesubstanz enthaltende Gefäß über die übrigen Gefäße hinweg zu transportieren. Das Fassungsvermögen der Trocknungskammer wird hierdurch erheblich reduziert. Weitere Probleme bereiten die in Verbindung mit einer Vakuumschleuse anfallenden dynamischen Dichtungen, die eine sorgfältige Wartung erforderlich machen.CORRECTED SHEET (RULE 81) ISA / EP a gripping mechanism is detected and the mass is removed during the freeze-drying process of the drying chamber for the purpose of determination. Continuous measurements or at least approximately continuous measurements are not possible here. In addition, this system is technically very complex, inter alia because of the necessary transport processes, and is also cost-intensive. This becomes particularly clear when a vessel containing a drying substance is not to be picked up at the edge of the shelf, but in the middle thereof, for the purpose of taking a sample, since a correspondingly large distance between the shelves is required in order to hold the vessel containing the sample substance over the other vessels to transport away. This significantly reduces the capacity of the drying chamber. The dynamic seals associated with a vacuum lock, which require careful maintenance, pose further problems.
Es ist die Aufgabe der Erfindung, eine Gefriertrock- nungsanlage der eingangs bezeichneten Art dahingehend auszugestalten , daß es möglich ist die Masse der in einzelnen Trocknungsgefäßen, z.B. Fläschchen oder son¬ stigen Gefäßen enthaltenen Trocknungssubstanz bei hoher Meßgenauigkeit wenigstens angenähert kontinuierlich zu bestimmen. Gelöst ist diese Aufgabe bei einer solchen Gefriertrocknungsanlage durch die Merkmale des Kenn¬ zeichnungsteils des Anspruchs 1.It is the object of the invention to design a freeze-drying system of the type mentioned in the introduction in such a way that it is possible to measure the mass of the individual drying vessels, e.g. To determine vials or other vessels containing drying substance at least approximately continuously with high measuring accuracy. This problem is solved in such a freeze drying system by the features of the characterizing part of claim 1.
Erfinduπgsweseπtlich ist hiernach eine Wägeeinrichtung, über welche die Masse eines auf einer Stellfläche mit direktem Kontakt aufstehenden Gefäßes unmittelbar meßbar ist. Dies bedeutet, daß für die Masse sämtlicher Gefäße in der gesamten Anlage einschließlich der zu wiegenden Masse zu jeder Zeit gleiche thermische und sonstigeAccording to the invention, a weighing device according to which the mass of a vessel standing on a shelf with direct contact can be measured directly is hereby. This means that for the mass of all vessels in the entire system, including the mass to be weighed, the same thermal and other at all times
BERICHTIGTES BLATT (REGEL 91) ISA/EP physikalische Bedingungen und damit gleiche Trocknungs¬ bedingungen vorherrschen und daß zur Durchführung des Wiegevorgangs der Gefriertrocknungsprozeß weder unter¬ brochen noch verändert wird. Das Meßergebnis ist somit als repräsentativ anzusehen. Die Wägeeinrichtung ist als elektrische Wägeeinrichtung ausgebildet, die ausgangs- seitig einen, der zu messenden Masse entsprechenden elektrischen Meßwert liefert, der in geeigneter Weise übertragbar und in externen Meß- und Auswertesystemen verarbeitbar ist. Letztere Übertragung kann über geeig¬ nete Meßleitungen erfolgen, die über vakuumdichte Durch¬ führungen durch die Wandung der Trocknungskammer verlegt sind. Es entfallen somit dynamische Dichtungen. Ein weiterer wesentlicher Vorteil dieses Systems besteht darin, daß der Meßvorgang nach Maßgabe der Dynamik des elektrischen Meßprinzips in kurzen Zeitabständen wieder¬ holt werden kann und auf diese Weise praktisch eine kontinuierliche Massenbestimmung und damit eine Kontrol¬ le des Ablaufs jeder Phase des Trocknungsprozesses möglich ist. So kann ein Meßwert der anfänglichen flüs¬ sigen Masse einschließlich derjenigen des Gefäßes mit dem Meßwert der Masse während des Trocknungsprozesses verglichen werden, wobei unter Berücksichtigung des Meßwertes der Trockenmasse und derjenigen des Gefäßes jeweils die Restfeuchte bestimmt werden kann. Die weite¬ re Auswertung dieses, die Masse der Trocknungssubstanz betreffenden Meßwertes kann in grundsätzlich beliebiger Weise erfolgen, d.h. auch zur Optimierung des Gefrier¬ trocknungsprozesses benutzt werden. Bei der Bildung des elektrischen Meßwertes können in einfacher Weise unter¬ schiedlichste thermische und sonstige physikalische Bedingungen des Meßvorgangs berücksichtigt werden, so daß die Meßgenauigkeit gewahrt ist.CORRECTED SHEET (RULE 91) ISA / EP physical conditions and thus the same drying conditions prevail and that the freeze-drying process is neither interrupted nor changed in order to carry out the weighing process. The measurement result can therefore be regarded as representative. The weighing device is designed as an electrical weighing device which, on the output side, supplies an electrical measured value corresponding to the mass to be measured, which can be transferred in a suitable manner and processed in external measuring and evaluation systems. The latter transmission can take place via suitable measuring lines, which are laid through vacuum-tight bushings through the wall of the drying chamber. This eliminates dynamic seals. Another important advantage of this system is that the measuring process can be repeated at short intervals in accordance with the dynamics of the electrical measuring principle, and in this way practically continuous mass determination and thus control of the course of each phase of the drying process is possible. In this way, a measured value of the initial liquid mass, including that of the vessel, can be compared with the measured value of the mass during the drying process, wherein the residual moisture can be determined taking into account the measured value of the dry mass and that of the vessel. The further evaluation of this measured value, which relates to the mass of the drying substance, can be carried out in any manner, that is, it can also be used to optimize the freeze-drying process. When forming the electrical measured value, a wide variety of different thermal and other physical conditions of the measuring process can be taken into account, so that the measuring accuracy is ensured.
Die Wägeeinrichtung besteht entsprechend den MerkmalenThe weighing device exists according to the characteristics
BERICHTIGTES BLATT (REGEL 91) ISA/EP des Anspruchs 2 aus einer Wägezelle, die über einenCORRECTED SHEET (RULE 91) ISA / EP of claim 2 from a load cell over a
Greifarm mit einem Gefäß in Verbindung steht. Auf einer Stellfläche befindet sich üblicherweise eine Vielzahl einzelner Gefäße und es besteht die Möglichkeit, eine oder mehrere derartiger Wägeeinrichtungen vorzusehen, die jeweils einer Stellfläche zugeordnet sind, um im Bedarfsfall mehrere Messungen - bezogen auf die Gefäße einer Stellfläche - durchführen zu können. Die Meßergeb¬ nisse können dann als repräsentativ für die Gesamtheit aller Gefäße einer Stellfläche angesehen werden. Grund¬ sätzlich kann eine Wägeeinrichtung bzw. eine Wägezelle auch mit mehreren Greifarmen ausgerüstet sein und somit zur gleichzeitigen oder aufeinander folgenden Bestimmung der Masse mehrerer Gefäße bestimmt und ausgestaltet sein.Gripper arm is connected to a vessel. There is usually a large number of individual vessels on a shelf and there is the possibility of providing one or more weighing devices of this type, each of which is assigned to a shelf, so that, if necessary, several measurements can be carried out in relation to the vessels of a shelf. The measurement results can then be regarded as representative of the totality of all the vessels in a footprint. In principle, a weighing device or a weighing cell can also be equipped with a plurality of gripping arms and can thus be determined and designed for the simultaneous or successive determination of the mass of a plurality of vessels.
Die Merkmale der Ansprüche 3 und 4 sind auf zwei unter¬ schiedliche Meßprinzipien gerichtet. Es kann hiernach die Wägezelle ortsfest in der Trocknungskammer oder in einer mit der Trocknungskammer in Verbindung stehenden Nebenkammer angeordnet sein, so daß zwecks Durchführung eines Meßvorgangs die Stellplatte, auf der das jeweilige Gefäß aufsteht, abgesenkt wird, so daß das zu wiegende Gefäß während des Meßvorgangs ausschließlich über den Greifarm gehalten ist. Es besteht jedoch auch die Mög- lichkeit, die Wägezelle mit einer Hubeinrichtuπg auszu¬ rüsten, über welche das Gefäß zwecks Durchführung des Meßvorgangs kurzfristig angehoben wird. Man erkennt, daß in jedem Fall der Meßvorgang kurzfristig und damit quasi kontinuierlich durchführbar ist und daß die Trocknungs- Substanz unter Bedingungen gemessen wird, die denjenigen der übrigen Gefäße einer Stellplatte entsprechen, so daß der Meßvorgang als repräsentativ für die Gesamtheit der jeweiligen Gefäße zumindest einer Stellplatte angesehen werden kann. Es können auf diese Weise praktisch gering- ste Mengen einer Trocknungssubstanz getrocknet werden und die zu messende Probe bleibt weiterhin benutzbar. Der Greifarm der Wägezelle ist zweckmäßigerweise derart ausgebildet, daß jede wählbare Stelle einer Stellfläche erreichbar ist, so daß auch insoweit sichergestellt ist, daß repräsentative Meßbedingungen eingehalten werden können .The features of claims 3 and 4 are directed to two different measuring principles. Thereafter, the load cell can be arranged in a stationary manner in the drying chamber or in a secondary chamber connected to the drying chamber, so that, for the purpose of carrying out a measuring process, the positioning plate on which the respective vessel stands is lowered so that the vessel to be weighed is during the measuring process is held exclusively over the gripper arm. However, there is also the possibility of equipping the load cell with a lifting device by means of which the vessel is raised briefly in order to carry out the measuring process. It can be seen that in each case the measuring process can be carried out briefly and thus quasi continuously, and that the drying substance is measured under conditions which correspond to those of the other vessels of a positioning plate, so that the measuring process is representative of the totality of the respective vessels at least one Stand plate can be viewed. In this way, maximum quantities of a drying substance are dried and the sample to be measured remains usable. The gripping arm of the load cell is expediently designed in such a way that every selectable position on a footprint can be reached, so that it is also ensured that representative measurement conditions can be maintained.
Das erfindungsgemäße Prinzip ist nicht davon abhängig, daß die Trocknungssubstanz in bestimmten Gefäßen gehal- ten ist - es können gleichermaßen auch Schalen, Fläsch¬ chen oder sonstige Trocknungsgefäße vorhanden sein, die die Trocknungssubstanz aufnehmen.The principle according to the invention is not dependent on the fact that the drying substance is held in certain vessels - bowls, vials or other drying vessels can also be present to hold the drying substance.
Die Erfindung wird im folgenden unter Bezugnahme auf das in der Zeichnung schematisch wiedergegebene Ausführungs- beispiel näher erläutert werden.The invention will be explained in more detail below with reference to the exemplary embodiment shown schematically in the drawing.
Die Zeichnung zeigt eine Gefriertrocknungsanlage, die global aus einer Trocknungskammer 1 und einer Kondensa¬ torkammer 2 besteht, welche über einen, mittels eines zeichnerisch nicht dargestellten Ventils schließbaren Durchgang 3 miteinander in Verbindung stehen. BeideThe drawing shows a freeze-drying system which consists globally of a drying chamber 1 and a condenser chamber 2 which are connected to one another via a passage 3 which can be closed by means of a valve (not shown in the drawing). Both
Kammern sind in dem gezeigten Ausführungsbeispiel neben¬ einander angeordnet - sie können jedoch gleichermaßen auch übereinander angeordnet sein. Auch kann der Konden¬ sator in die Trocknungskammer eingebaut sein.In the exemplary embodiment shown, chambers are arranged next to one another - however, they can equally well be arranged one above the other. The capacitor can also be installed in the drying chamber.
Mit 4 ist ein Wärmetauscher innerhalb der Kondensator¬ kammer bezeichnet, der die Funktion eines Eiskondensa¬ tors hat und in einen, unter anderem eine Kältemaschine 5 beinhaltenden Kältemittelkreislauf 6 eingebunden ist. Die Kondensatorkammer 2 steht darüber hinaus über eine Leitung 7 mit einem Vakuumerzeuger 0 in Verbindung. Die Trocknungskammer beinhaltet unter anderem ein System von übereinander angeordneten Stellplatten 9, die in eine, in der Zeichnung nicht näher dargestellte Füh- rungs- oder Verschiebeeinrichtung eingesetzt sind und in dieser in Richtung der Pfeile 10, somit senkrecht zu ihrer Ebene verschiebbar sind. Die Verschiebung erfolgt derart, daß sich der Abstand zwischen sämtlichen Stell¬ platten 9 auf diese Weise verringern läßt.4 denotes a heat exchanger within the condenser chamber, which has the function of an ice condenser and is integrated in a refrigerant circuit 6, which includes a refrigeration machine 5, among other things. The condenser chamber 2 is also connected via a line 7 to a vacuum generator 0. The drying chamber contains, among other things, a system of stacking plates 9 arranged one above the other, which are inserted into a guide or displacement device (not shown in the drawing) and can be displaced in the direction of the arrows 10, thus perpendicular to their plane. The displacement takes place in such a way that the distance between all the setting plates 9 can be reduced in this way.
Die Verschiebung wird über eine Druckplatte 11 ausge- löst, die mit einem schematisch dargestellten Antrieb 12 in zeichnerisch nicht näher dargestellter Verbindung steht. Der Antrieb 12 befindet sich in dem Ausführungs¬ beispiel unterhalb der Trocknungskammer. Er kann jedoch auch oberhalb der Trocknungskammer angeordnet sein. Der Antrieb 12 kann beispielsweise als eine, beidseitig mit einem Druckmittel beaufschlagbare Kolben-Zylinder-Ein¬ heit ausgestaltet sein. Hierauf soll jedoch im weiteren nicht näher eingegangen werden.The displacement is triggered by a pressure plate 11 which is connected to a schematically illustrated drive 12 in a connection not shown in the drawing. In the exemplary embodiment, the drive 12 is located below the drying chamber. However, it can also be arranged above the drying chamber. The drive 12 can be configured, for example, as a piston-cylinder unit to which pressure medium can be applied on both sides. However, this will not be discussed further below.
Die Stellplatten 9 können in an sich bekannter Weise temperierbar ausgebildet sein und dienen als Stellflä¬ chen für Fläschchen 13, die beispielsweise über Vaku¬ umstopfen 14 verschlossen sind. Diese Fläschchen bein¬ halten die Trocknungssubstanz, wobei die genannten Stopfen die Eigenschaft haben, im lose aufgesetzten Zustand ein Entweichen von Dämpfen aus der Trocknungs¬ substanz zu ermöglichen, im eingedrückten Zustand hinge¬ gen das Fläschchen 13 vakuumdicht zu verschließen.The setting plates 9 can be designed to be temperature-controlled in a manner known per se and serve as setting surfaces for vials 13, which are closed, for example, by means of vacuum plugs 14. These vials contain the drying substance, the stoppers mentioned having the property of allowing vapors to escape from the drying substance in the loosely attached state, but sealing the vial 13 in a vacuum-tight manner when pressed in.
Zur Durchführung des TrocknungsVorgangs werden die Fläschchen 13 mit lose aufgesetzten Vakuumstopfen in die, beispielsweise vorderseitig mit einer verschließba¬ ren Öffnung versehene Trocknungskammer 1 eingesetzt, wobei nach vollendetem Trocknungs organg durch Betäti- gung des Antriebs 12 das System der Stellplatten 9 derart bewegt wird, daß sich die Platten aufeinander zubewegen, so daß auf diese Weise die Vakuumstopfen in die Fläschchen 13 hineingedrückt werden, um diese vaku- umdicht zu verschließen.To carry out the drying process, the vials 13 are inserted with loosely placed vacuum plugs into the drying chamber 1, for example provided with a closable opening on the front. tion of the drive 12, the system of the setting plates 9 is moved in such a way that the plates move towards one another, so that in this way the vacuum plugs are pressed into the bottles 13 in order to close them in a vacuum-tight manner.
Erfindungsgemäß sind an bzw. in der Trocknungskammer 1 Wägezellen 15 angeordnet, die vorzugsweise auf einem elektrischen Meßprinzip beruhen und über zeichnerisch nicht dargestellte Meßleitungen mit einer übergeordneten Steuerung, einem PC oder dergleichen in Verbindung stehen. Jede dieser Wägezellen steht über einen, an ihre jeweilige Anordnung innerhalb oder an der Trocknungskam¬ mer 1 angepaßten Greifarm 16 mit einem Fläschchen 13 in Verbindung, wobei die unmittelbare Verbindung des Greif- arms 16 mit dem Fläschchen 13 an dessen spezielle Geome¬ trie in zeichnerisch nicht dargestellter Weise angepaßt ist.According to the invention, load cells 15 are arranged on or in the drying chamber 1, which are preferably based on an electrical measuring principle and are connected to a higher-level control, a PC or the like via measuring lines (not shown in the drawing). Each of these load cells is connected to a vial 13 via a gripping arm 16, which is adapted to their respective arrangement inside or on the drying chamber 1, the direct connection of the gripping arm 16 to the vial 13 at its special geometry being shown in the drawing is not shown adapted.
In einem ersten Fall befindet sich die Wägezelle 15 auf der oberen, gegenüber den Wandungen der Trocknungskammer 1 unbeweglichen Druckplatte 11' , wobei der Greifarm 16 ein Fläschchen 13 auf der unmittelbar darunter liegenden Stellplatte 9 erfaßt. Ein Wägevorgang kann in diesem Fall derart durchgeführt werden, daß die Stellplatte 9 abgesenkt wird, so daß das Fläschchen ausschließlich an dem Greifarm 16 hängt. Grundsätzlich kann auch über die Wägezelle 15 bei unveränderter Position der Stellplatte 9 über den Greifarm 16 das Fläschchen 13 kurzfristig angehoben werden.In a first case, the load cell 15 is located on the upper pressure plate 11 ', which is immovable relative to the walls of the drying chamber 1, the gripping arm 16 gripping a vial 13 on the positioning plate 9 located immediately below it. In this case, a weighing process can be carried out in such a way that the setting plate 9 is lowered so that the vial hangs exclusively on the gripping arm 16. In principle, the vial 13 can also be raised briefly via the load cell 15 with the position of the positioning plate 9 unchanged via the gripping arm 16.
In einem anderen Fall befindet sich die Wägezelle 15 unmittelbar neben dem zu wiegenden Fläschchen 13 auf einer Stellplatte 9. In diesem Fall kann der Wägevorgaπg nur über ein kurzfristiges Anheben des Fläschchens 13 bewirkt werden.In another case, the weighing cell 15 is located directly next to the vial 13 to be weighed on a positioning plate 9. In this case, the weighing operation can only be done by briefly lifting the vial 13 be effected.
Die Wägezelle 15 kann auch ortsfest innerhalb der Trock¬ nungskammer 1 beispielsweise auf einer Konsole, Platt¬ form oder dergleichen untergebracht werden, wobei ein Wägevorgang wiederum entsprechend den beiden oben darge¬ legten grundsätzlichen Varianten durchführbar ist.The weighing cell 15 can also be accommodated in a stationary manner within the drying chamber 1, for example on a console, platform or the like, a weighing process in turn being able to be carried out in accordance with the two basic variants set out above.
Schließlich kann die Wägezelle 15 auch in einer Neben¬ kammer 17 angeordnet sein, die über einen Verbindungska¬ nal 18 an die Trocknungskammer 1 angeschlossen ist, wobei der Verbindungskanal 18 der Aufnahme des Greifarms 16 dient. Auch in diesem Fall kann der Wägevorgang nach den beiden oben bereits dargelegten Prinzipien durchge¬ führt werden.Finally, the load cell 15 can also be arranged in a secondary chamber 17, which is connected to the drying chamber 1 via a connecting channel 18, the connecting channel 18 serving to receive the gripping arm 16. In this case too, the weighing process can be carried out according to the two principles already outlined above.
Wesentlich ist, daß entsprechend der elektrischen Ausge- staltung der Wägezellen der Wägevorgang sehr schnell durchführbar ist, und zwar ohne daß als Folge des Me߬ vorgangs in den TrocknungsVorgang eingegriffen werden muß. Dies ermöglicht in Verbindung mit einem schnellen Meßvorgang eine zu beliebigen Zeiten wiederholbare Messung, so daß auf diesem Wege der Trocknungsprozeß praktisch kontinuierlich kontrollierbar wird, so daß z.B. Aussagen über den Masseverlust pro Zeiteinheit - ausgehend vom flüssigen bis zum fertig getrockneten Zustand des Produktes - in der jeweiligen Gefriertrock- nungsphase möglich sind und auch der Einfluß von anderen Prozeßgrößen des Trocknungsvorgangs wie z.B. Druck und Temperatur, jedoch auch von sonstigen konstruktiven Parametern der Trocknungsanlage wie z.B. unterschiedli¬ chen Strömungsquerschnitten des die Trocknungskammer 1 mit der Kondensatorkammer 2 verbindenden Durchgangs 3 bzw. der Stellung des hier angeordneten Ventils unter¬ sucht werden können. Bereits während der Gefriertrock- nung kann sowohl der Restfeuchteanteil im Produkt als auch das Ende des Gefriertrocknungsprozesses bei einer bestimmten Restfeuchte ermittelt werden.It is essential that, according to the electrical design of the load cells, the weighing process can be carried out very quickly, without having to intervene in the drying process as a result of the measuring process. In connection with a fast measuring process, this enables a repeatable measurement at any time, so that the drying process can be practically continuously monitored in this way, so that, for example, statements about the mass loss per unit of time - starting from the liquid to the completely dried state of the product - in the freeze drying phase are possible and also the influence of other process variables of the drying process, such as pressure and temperature, but also of other design parameters of the drying system, such as different flow cross sections of the passage 3 connecting the drying chamber 1 to the condenser chamber 2 or the position of the valve arranged here can be examined. Already during the freeze drying Both the residual moisture content in the product and the end of the freeze-drying process at a certain residual moisture can be determined.
Bei entsprechend kurzen Meßvorgängen ist auf diesem Wege eine angenähert kontinuierliche Massebestimmung derWith correspondingly short measuring processes, an approximately continuous mass determination of the
Trocknungssubstanz in jeder Phase der Gefriertrocknung möglich .Drying substance possible in every phase of freeze drying.
Das Meßergebπis liegt am Ausgang der Wägezellen zweckmä¬ ßigerweise in digital kodierter Form vor, so daß über entsprechend gestaltete Schnittstellen eine unmittelbare Einspeisung in eine EDV-Anlage zwecks weitergehenderer Auswertung möglich ist. The measurement result is expediently available in digitally coded form at the output of the load cells, so that it can be fed directly into an EDP system for further evaluation via appropriately designed interfaces.

Claims

P A T E N T A N S P R Ü C H E PATENT CLAIMS
1. Gefriertrocknungsanlage, bestehend aus einer Konden¬ sator- (2) und einer Trocknungskammer (1) , wobei die Trocknungskammer (1) ein System von zueinander paral- lelen, übereinander angeordneten, horizontale Stell¬ flächen aufweisenden Stellplatten (9) beinhaltet und wobei sich auf den Stellflächen Gefäße befinden, die der Aufnahme einer Trocknungssubstanz dienen, dadurch gekennzeichnet,1. Freeze-drying system, consisting of a condenser (2) and a drying chamber (1), the drying chamber (1) containing a system of parallel, one above the other, horizontal standing surfaces with standing plates (9) and wherein there are vessels on the shelves which serve to hold a drying substance, characterized in that
- daß die Trocknungskammer (1) mit wenigstens einer, eine Massebestimmung eines auf einer Stellplatte (9) aufstehenden Gefäßes ermöglichenden Wägeein¬ richtung ausgerüstet ist und- That the drying chamber (1) is equipped with at least one weighing device which enables a mass determination of a vessel standing on a positioning plate (9) and
- daß die Wägeeiπrichtung zur Bildung und Übertragung eines der zu messenden Masse entsprechenden elek¬ trischen Meßwertes ausgestaltet ist.- The weighing device is designed to form and transmit an electrical measured value corresponding to the mass to be measured.
2. Gefriertrocknungsanlage nach Anspruch 1, dadurch gekennzeichnet, daß die Wägeeinrichtung aus einer Wägezelle (15) besteht, die über einen Greifarm (16) mit einem Gefäß in Verbindung steht.2. Freeze drying system according to claim 1, characterized in that the weighing device consists of a load cell (15) which is connected to a vessel via a gripping arm (16).
3. Gefriertrocknungsanlage nach Anspruch 2, dadurch gekennzeichnet , - daß die Wägezelle (15) in der Trocknungskammer (1) gegenüber der das Gefäß tragenden Stellplatte (9) ortsfest angeordnet ist und3. Freeze drying system according to claim 2, characterized in - That the load cell (15) in the drying chamber (1) with respect to the support plate supporting the vessel (9) is arranged stationary and
- daß diese Stellplatte (9) gegenüber der Wägezelle (15) beweglich angeordnet ist.- That this adjusting plate (9) relative to the load cell (15) is movably arranged.
4. Gefriertrocknungsanlage nach Anspruch 2, dadurch gekennzeichet ,4. Freeze drying system according to claim 2, characterized gekennzeichet
- daß die Wägezelle (15) eine Hubeinrichtung beinhal¬ tet, über welche das Gefäß zwecks Massebestimmuπg gegenüber der jeweiligen Stellplatte (S) anhebbar ist . - That the load cell (15) includes a lifting device, by means of which the vessel can be raised relative to the respective setting plate (S) for the purpose of determining the mass.
PCT/EP1994/002426 1993-10-13 1994-07-22 Freeze-drying plant WO1995010744A1 (en)

Priority Applications (2)

Application Number Priority Date Filing Date Title
DE59404209T DE59404209D1 (en) 1993-10-13 1994-07-22 FREEZER DRYING SYSTEM
EP94924796A EP0672234B1 (en) 1993-10-13 1994-07-22 Freeze-drying plant

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE4334902A DE4334902C2 (en) 1993-10-13 1993-10-13 Freeze dryer
DEP4334902.1 1993-10-13

Publications (1)

Publication Number Publication Date
WO1995010744A1 true WO1995010744A1 (en) 1995-04-20

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EP (1) EP0672234B1 (en)
DE (2) DE4334902C2 (en)
DK (1) DK0672234T3 (en)
WO (1) WO1995010744A1 (en)

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DE102005024536A1 (en) * 2005-05-28 2006-11-30 Hans-Georg Hof Horizontal freeze-drying plant
DE102012007422B4 (en) 2012-04-16 2024-02-08 Martin Christ Gefriertrocknungsanlagen Gmbh Process for freeze-drying substances and system for carrying out this process
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Also Published As

Publication number Publication date
DE59404209D1 (en) 1997-11-06
DE4334902A1 (en) 1995-04-20
DE4334902C2 (en) 1998-07-02
DK0672234T3 (en) 1997-12-08
EP0672234B1 (en) 1997-10-01
EP0672234A1 (en) 1995-09-20

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