EP1412686B1 - Chamber for a freeze-drying device - Google Patents

Chamber for a freeze-drying device Download PDF

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Publication number
EP1412686B1
EP1412686B1 EP20020791452 EP02791452A EP1412686B1 EP 1412686 B1 EP1412686 B1 EP 1412686B1 EP 20020791452 EP20020791452 EP 20020791452 EP 02791452 A EP02791452 A EP 02791452A EP 1412686 B1 EP1412686 B1 EP 1412686B1
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EP
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Prior art keywords
chamber
plates
temperature
components
drying
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EP20020791452
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German (de)
French (fr)
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EP1412686A1 (en
EP1412686B8 (en
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Peter Haseley
Georg-Wilhelm Oetjen
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GEA Lyophil GmbH
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GEA Lyophil GmbH
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Priority to DE2001136498 priority patent/DE10136498A1/en
Application filed by GEA Lyophil GmbH filed Critical GEA Lyophil GmbH
Priority to PCT/EP2002/007828 priority patent/WO2003012355A1/en
Publication of EP1412686A1 publication Critical patent/EP1412686A1/en
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    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F26DRYING
    • F26BDRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
    • F26B5/00Drying solid materials or objects by processes not involving the application of heat
    • F26B5/04Drying 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
    • F26B5/06Drying 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

Description

  • Die Erfindung bezieht sich auf eine Kammer für eine Gefriertrocknungseinrichtung mit den Merkmalen des Oberbegriffs des Patentanspruchs 1.The invention relates to a chamber for a freeze-drying device with the features of the preamble of patent claim 1.
  • Die Gefriertrocknung hat sich insbesondere in der pharmazeutischen Industrie zur Konservierung von Medikamenten, Impfstoffen usw. durchgesetzt. In den Kammern moderner Gefriertrocknungseinrichtungen befindet sich eine Mehrzahl von Stellplatten, auf deren Stellflächen eine Vielzahl von Behältern, Fläschchen o.dgl. (100.000 und mehr) Platz findet. Das üblicherweise in Wasser gelöste Produkt wird in Behälter dieser Art gefüllt. Vor dem Beginn des Gefriertrocknungsprozesses erfolgt das Einfrieren der Flüssigkeit. Üblicherweise findet dieser Schritt bereits in der Kammer der Gefriertrocknungseinrichtung statt, indem die Stellflächen entsprechend tief (-40° C bis -60° C) gekühlt werden.Freeze-drying has prevailed particularly in the pharmaceutical industry for the preservation of medicines, vaccines, etc. In the chambers of modern freeze-drying facilities is a plurality of parking plates on the shelves a variety of containers, vials or the like. (100,000 and more) takes place. The product, usually dissolved in water, is filled into containers of this type. Before the start of the freeze-drying process, the freezing of the liquid takes place. Usually, this step takes place already in the chamber of the freeze-drying device by the shelves are correspondingly deep (-40 ° C to -60 ° C) cooled.
  • Aus der deutschen Offenlegungsschrift 197 19 298 ist eine Kammer der eingangs erwähnten Art bekannt. Außerdem wird in diesem Dokument ein Verfahren zur Steuerung des Gefriertrocknungsprozesses in der Kammer erläutert. Kennzeichnend für den Ablauf des Trocknungsprozesses sind im wesentlichen zwei Trocknungsphasen. Solange sich noch kristallisiertes (gefrorenes) Wasser in dem Produkt befindet, nennt man diesen Trockenabschnitt die Haupt- oder Sublimationstrocknung. Liegt kein Wasser in Form von Eis mehr vor, ist das restliche Wasser am Trockenprodukt absorbiert und auch mehr oder weniger fest gebunden. Die Entfernung dieses Wassers findet während der Nach- oder Desorptionstrocknung statt. Zur Steuerung eines Gefriertrocknungsprozesses dieser Art werden bestimmte Kammerdrücke und Stellflächentemperaturen eingestellt. Ein wesentlicher Parameter ist dabei die Eistemperatur, die durch Druckanstiegsmessungen bestimmbar ist.From the German patent application 197 19 298 a chamber of the type mentioned is known. In addition, this document describes a method of controlling the freeze-drying process in the chamber. Characteristic of the course of the drying process are essentially two drying phases. As long as there is crystallized (frozen) water in the product, this drying section is called the main or sublimation drying. If there is no more water in the form of ice, the remaining water is absorbed on the dry product and also more or less firmly bound. The removal of this water takes place during the desorption or desorption drying. To control a freeze-drying process of this type, certain chamber pressures and shelf temperatures are used set. An essential parameter is the ice temperature, which can be determined by pressure increase measurements.
  • Die Steuerung der Eistemperatur in der Sublimationsfläche über den Druck setzt voraus, dass ein gleichförmiger Wasserdampfpartialdruck in der Kammer herrscht. Diese gleichförmige Druckverteilung ist im Bereich der Kammerwände sowie Kammertür oder -türen nur begrenzt möglich. In diesen Bereichen hängt die Temperatur des in den Fläschchen befindlichen Produkts nicht nur von der Stellplattentemperatur ab; auch die Temperatur der Innenwände der Kammer wirkt sich über Wärmestrahlung aus. Hat z.B. der aus dem Produkt austretende Wasserdampf eine Temperatur von -40°C, dann erhöht sich diese Temperatur auf den Stellplatten z.B. auf -20° C, während der Wasserdampf in der Nähe der Wände z.B. 20°C erreicht. Aufgrund dieser Temperaturunterschiede können sich Druckunterschiede von mehr als 10% einstellen. Die gewünschte Voraussetzung, dass ein gleichmäßiger Wasserdampfpartialdruck in der Kammer herrscht, ist nicht mehr ausreichend genau erfüllt; die sich einstellende Eistemperatur ist nicht mehr gleichförmig. Einbußen der Produktqualität sind die Folge.The control of the ice temperature in the sublimation surface above the pressure presupposes that there is a uniform water vapor partial pressure in the chamber. This uniform pressure distribution is limited in the area of the chamber walls and chamber door or doors possible. In these areas, the temperature of the product in the vial does not only depend on the platen temperature; The temperature of the inner walls of the chamber also has an effect on thermal radiation. Has e.g. the water vapor exiting the product reaches a temperature of -40 ° C, then this temperature increases on the control panels e.g. at -20 ° C, while the water vapor near the walls e.g. 20 ° C reached. Due to these temperature differences, pressure differences of more than 10% can occur. The desired condition that a uniform water vapor partial pressure prevails in the chamber, is no longer met with sufficient accuracy; the resulting ice temperature is no longer uniform. Loss of product quality are the result.
  • Um den Einfluss der Kammerwandtemperatur auf die Temperatur des in den Fläschchen befindlichen Produkts zu vermeiden, ist es bekannt, die Stellplatten mit einem äußeren Rand auszurüsten, der das Produkt vor einer von den Kammerwänden ausgehenden Wärmestrahlung schützt. Diese Maßnahmen haben jedoch nur einen begrenzten Erfolg gehabt, da die Temperaturunterschiede zwischen dem Rand und den Stellflächen ca. 20°C betragen.In order to avoid the influence of the chamber wall temperature on the temperature of the product in the vial, it is known to provide the control panels with an outer edge which protects the product from heat radiation emanating from the chamber walls. However, these measures have had only a limited success, since the temperature differences between the edge and the shelves are about 20 ° C.
  • Weiterhin wurde bereits vorgeschlagen, die Wände und Tür(en) der Kammer zu temperieren. Diese Maßnahmen sind jedoch mit praktisch unüberwihdbaren technischen Schwierigkeiten und wirtschaftlichen Nachteilen verbunden. Die Kammer mit ihrer (ihren) Tür(en) kann bei Produktionsanlagen, besonders wenn sie mit Dampf sterilisiert werden müssen, eine Masse von vielen Tonnen haben. Diese Massen müssten bis -40°C und oft bis -60°C beim Einfrieren abgekühlt werden, was entweder zu einer unzulässig langen Einfrierzeit führt oder zu getrennten Kühlsystemen, die ein mehrfaches an Kälteleistung abgeben müssen, als sie für die Stellplatten und das Produkt erforderlich ist. Abgesehen von diesen wirtschaftlichen Problemen ist es technisch schwierig, die Flansche an der Kammer und den Flansch an der Tür auf z.B. -50°C zu kühlen. Die Dichtungen zwischen Kammer und Tür müssen bei tiefen Temperaturen funktionsfähig bleiben, und es ist schwierig, ein Kondensieren des Wasserdampfes an diesen Flanschen zu vermeiden. Eine denkbare Isolierung der Flansche gegen die Wasserdampfkondensation ist technisch nicht möglich, da Kammerflansch und Tür in sterilen Räumen untergebracht sind. Die Sterilitätsanforderungen in einem Reinraum schließen die Verwendung von für diese tiefen Temperaturen geeigneten Isoliermaterialien aus. Gefriertrocknungskammern nach dem Oberbegriff des Patentanspruchs 1 sind aus den US-Patentschriften 30 48 92 und 3 311 911 bekannt.Furthermore, it has been proposed to temper the walls and door (s) of the chamber. However, these measures are associated with practically unattainable technical difficulties and economic disadvantages. The chamber with its door (s) can be used in production plants, especially if they need to be steam sterilized, have a mass of many tons. These masses would have to be cooled down to -40 ° C and often down to -60 ° C during freezing, resulting either in an inadmissibly long freezing time or in separate cooling systems which have to give off more cooling power than required for the control panels and the product is. Apart from these economic problems, it is technically difficult to cool the flanges on the chamber and the flange on the door to eg -50 ° C. The gaskets between the chamber and the door must remain functional at low temperatures, and it is difficult to avoid condensing the water vapor at these flanges. A conceivable insulation of the flanges against the condensation of water vapor is technically not possible because chamber flange and door are housed in sterile rooms. The sterility requirements in a clean room preclude the use of insulating materials suitable for these low temperatures. Freeze-drying chambers according to the preamble of claim 1 are known from US Pat. Nos. 3,048,992 and 3,311,911.
  • Beim Gegenstand der US-PS 30 48 928 ist eine innere Stellplatte 25 von einem inneren Container 13 mit Öffnungen 18 umgeben. Innerhalb des Containers 13 wird die für die Gefriertrocknung notwendige Energie mit Hilfe von Mikrowellen erzeugt. Die Wandungen des Containers 13 dienen der Abschirmung der Mikrowellen.In the subject of US-PS 30 48 928 an inner control plate 25 is surrounded by an inner container 13 with openings 18. Within the container 13, the energy required for freeze-drying is generated by means of microwaves. The walls of the container 13 serve to shield the microwaves.
  • Beim Gegenstand der US-PS 3 311 911 haben die plattenförmigen Bauteile 16, die sich zwischen den Stellplatten 12 und den Innenwandflächen der Kammer 10 befinden, Kondensatorfunktion. Die Kühlung der Platten 16 erfolgt dadurch, daß eine gekühlte, Wasserdampf absorbierende Flüssigkeit über die Oberflächen der Platten strömt.In the subject matter of US-PS 3 311 911, the plate-shaped components 16, which are located between the adjusting plates 12 and the inner wall surfaces of the chamber 10, capacitor function. The cooling of the plates 16 is accomplished by flowing a cooled, water vapor-absorbing liquid over the surfaces of the plates.
  • Der vorliegenden Erfindung liegt die Aufgabe zugrunde, eine Kammer für eine Gefriertrocknungseinrichtung der eingangs erwähnten Art ohne besonderen technischen Aufwand so auszubilden, dass sich während des Gefriertrocknungsprozesses gleichförmige Temperatur- und Wasserdampfdruckverhältnisse einstellen.The present invention has for its object, a chamber for a freeze-drying device of the type mentioned without special technical effort in such a way that set during the freeze-drying process uniform temperature and water vapor pressure conditions.
  • Erfindungsgemäß wird diese Aufgabe durch die kennzeichnenden Merkmale der Patentansprüche gelöst.According to the invention this object is achieved by the characterizing features of the claims.
  • Die aus temperierbaren Bauteilen bestehende optische Abschirmung befindet sich zwischen den Stellflächen und den Kammerinnenflächen. Während der Durchführung des Gefriertrocknungsprozesses werden die temperierbaren Bauteile jeweils auf die Temperatur eingestellt, die auch die Stellplatten haben. Die Kammerwandtemperaturen können die Temperatur des in den Fläschchen befindlichen Produkts nicht mehr beeinflussen. In dem von den Abschirmbauteilen begrenzten Innenraum herrschen keine messbaren Temperatur- und Wasserdampfdruckunterschiede mehr.The consisting of temperature-controllable components optical shield is located between the shelves and the chamber inner surfaces. During the execution of the freeze-drying process, the temperature-controllable components are each set to the temperature which also has the control plates. The chamber wall temperatures can no longer affect the temperature of the product in the vial. In the limited by the Abschirmbauteilen interior no measurable temperature and water vapor pressure differences prevail.
  • Weitere Vorteile und Einzelheiten der Erfindung sollen anhand eines in den Figuren 1 und 2 schematisch dargestellten Ausführungsbeispieles erläutert werden. Es zeigen
    • Figur 1 einen Vertikalschnitt durch eine Kammer nach der Erfindung,
    • Figur 2 einen Horizontalschnitt durch diese Kammer.
    Further advantages and details of the invention will be explained with reference to an embodiment shown schematically in Figures 1 and 2. Show it
    • 1 shows a vertical section through a chamber according to the invention,
    • Figure 2 is a horizontal section through this chamber.
  • In den Figuren sind die Kammer mit 1, die Kammerwandung mit 2, ihre Tür mit 3 (Figur 2), die in der Kammer 1 befindlichen Stellplatten mit 4 und ein beispielhaft dargestelltes, auf der Stellfläche einer Stellplatte 4 abgesetztes Fläschchen mit 5 bezeichnet. Die untere Stellplatte 4 stützt sich auf einer ortsfesten Basisplatte 6 ab. Die übrigen Stellplatten 4 sind derart auf- und abbewegbar (Doppelpfeil 7), dass sich ihr Abstand verändert. Durch ein Zusammenfahren der Stellplatten z.B. mit Hilfe eines hydraulischen Antriebs (Kolbenstange 8) erfolgt in bekannter Weise das Verschließen der Fläschchen 5 mit Stopfen, die seitlich endende Durchtrittskanäle für den Wasserdampf aufweisen und vor dem Beginn des Gefriertrocknungsprozesses auf die Fläschchen 5 aufgesetzt werden. Die oberste Stellplatte 4 ist am Stempel 9 der Kolbenstange 8 befestigt.In the figures, the chamber with 1, the chamber wall with 2, their door with 3 (Figure 2), located in the chamber 1 with 4 Stellplatten and an exemplified, on the footprint of a control plate 4 deposed vial with 5 are designated. The lower adjusting plate 4 is supported on a stationary base plate 6. The other control panels 4 are moved up and down (double arrow 7) that changed their distance. By moving together the control panels e.g. by means of a hydraulic drive (piston rod 8) is carried out in a known manner, the closure of the vials 5 with plugs which have laterally ending passageways for the water vapor and are placed on the vial 5 before the beginning of the freeze-drying process. The uppermost adjusting plate 4 is fixed to the punch 9 of the piston rod 8.
  • Die Stellplatten 4 sind Bestandteil eines gestrichelt angedeuteten Temperierkreislaufs 11. Er ist von einer Sole durchströmt, die je nach Bedarf in einen Wärmetauscher 12 (angeschlossen an eine nicht dargestellte Kältemaschine) gekühlt oder mit einer Heizung 13 aufgeheizt wird. Dem gesteuerten Ablauf des Gefriertrocknungsprozesses dient eine als Block dargestellte Steuerung 15, der als Steuergröße u.a. Signale eines in der Kammer angeordneten Drucksensors 16 zugeführt werden. Zu Beginn des Gefriertrocknungsprozesses werden die Stellplatten zunächst gekühlt (Einfrierphase). Während der Trocknungsphasen haben die Stellplatten Temperaturen über 0°C, um den Verdampfungsprozess zu beschleunigen.He is traversed by a brine, which is cooled as needed in a heat exchanger 12 (connected to a chiller, not shown) or heated with a heater 13. The controlled process of the freeze-drying process is a control 15 shown as a block, which are supplied as a control variable, inter alia, signals of a pressure sensor 16 arranged in the chamber. At the beginning of the freeze-drying process, the shelves are first cooled (freezing phase). During the Drying phases have the shelves temperatures above 0 ° C to accelerate the evaporation process.
  • Die Kammer 1 ist mit einem Anschlussstutzen 21 ausgerüstet, an den über ein Ventil 22 ein Kondensator 23 und eine Vakuumpumpe 24 angeschlossen sind. Der Kondensator 23 dient der Anlagerung des Wasserdampfes, der während der Gefriertrocknung anfällt. Nicht kondensierbare Gase werden von der Vakuumpumpe 24 entfernt. Das Ventil 22 steht mit der Steuerung 15 in Verbindung. Es wird zeitweise geschlossen, um mit Hilfe von Druckanstiegsmessungen die Eistemperatur bestimmen zu können.The chamber 1 is equipped with a connecting piece 21 to which a valve 22, a capacitor 23 and a vacuum pump 24 are connected. The condenser 23 serves to accumulate the water vapor which accumulates during freeze-drying. Non-condensable gases are removed from the vacuum pump 24. The valve 22 is in communication with the controller 15. It is temporarily closed in order to be able to determine the ice temperature with the aid of pressure increase measurements.
  • Um das erfindungsgemäße Ziel zu erreichen, ist eine Abschirmung zwischen den Stellflächen und den Innenflächen der Kammerwand 2 vorgesehen. Sie besteht aus mehreren Bauteilen 31 bis 36, die die Stellplatten 4 derart umfassen, dass keine Sichtverbindung zwischen den Stellflächen und den darauf abgesetzten Fläschchen5 einerseits und den Kammerinnenwandflächen andererseits besteht. Die zwischen den Bauteilen gewählten Abstände sind so groß bemessen, dass der Wasserdampftransport zwischen den Stellflächen und dem Anschlussstutzen 21 im wesentlichen ungehindert stattfinden kann. Zweckmäßig ist es deshalb, wenn sich die einzelnen Bauteile nach Art einer Jalousie überlappen.In order to achieve the object of the invention, a shield between the shelves and the inner surfaces of the chamber wall 2 is provided. It consists of several components 31 to 36, which include the adjusting plates 4 such that there is no line of sight between the shelves and the vials deposited thereon on the one hand and the chamber inner wall surfaces on the other. The distances chosen between the components are dimensioned so large that the transport of water vapor between the shelves and the connecting piece 21 can take place substantially unhindered. It is useful, therefore, if the individual components overlap in the manner of a blind.
  • Beim dargestellten Ausführungsbcispiel umfassen die Bauteile 31 bis 36 das Stellplattenpaket von allen Seiten. Nach oben und nach unten bilden die obere bzw. untere Stellplatte 4 den erwünschten, temperierten Sichtschutz. Ist z.B. eine obere Stellplatte 4 nicht vorhanden, müssen ein oder mehrere weitere Bauteile vorhanden sein, die für die optische Abschirmung zur oberen Kammerwandung hin sorgen.In the illustrated embodiment, the components 31 to 36 comprise the set plate package from all sides. Upwards and downwards form the upper and lower control plate 4 the desired tempered screen. For example, if an upper control plate 4 is not present, one or more other components must be present, which provide for the optical shield to the upper chamber wall out.
  • Durch die erfindungsgemäßen Bauteile entsteht ein innerer, nach außen optisch dichter Raum 37, in dem sich die Stellplatten 4 bzw. Stellflächen für die Fläschchen 5 befinden. Von den Kammerinnenwandflächen ausgehende Strahlungswärme kann die Temperatur- und Druckverhältnisse im Raum 37 nicht mehr beeinflussen. Während des Ablaufs des Gefriertrocknungsprozesses stellen sich die gewünschten Drücke und Temperaturen im Raum 37 gleichmäßig ein.By the components according to the invention an inner, visually dense outside space 37, in which the adjusting plates 4 and shelves for the vials 5 are. Radiant heat emanating from the chamber inner wall surfaces can no longer influence the temperature and pressure conditions in the space 37. During the course of the freeze-drying process, the desired pressures and temperatures in the space 37 are uniform.
  • Um eine optimale Abschirmung der Stellflächen auch in Kantenbereichen des Stellplattenpaketes zu erreichen, weisen die Bauteile 31, 32 oben und unten abgebogene.Endabschnitte auf. Eine Alternative dazu zeigt Figur 2. Im Bereich der hinteren Kanten des Stellplattenpaketes enden die Bauteile 31, 33 bzw. 32, 33 jeweils mit einem den Dampfdurchtritt nicht behindernden Spalt. Den Spalten sind mit ausreichendem Abstand weitere Bauteile 34, 35, vorzugsweise zwischen den Spalten und der Kammerwand 2, zugeordnet, deren Breite und Länge so gewählt sind, dass eine Sichtverbindung zwischen den Stellflächen und der Kammerinnenwand durch die Spalte hindurch nicht besteht.In order to achieve optimum shielding of the shelves in edge regions of the set of parking plates, the components 31, 32 have bent end sections at the top and bottom. An alternative to this is shown in FIG. 2. In the region of the rear edges of the set of parking plates, the components 31, 33 or 32, 33 end in each case with a gap which does not hinder the passage of steam. The columns are at a sufficient distance other components 34, 35, preferably between the columns and the chamber wall 2, assigned, whose width and length are chosen so that a line of sight between the shelves and the chamber inner wall through the column does not exist.
  • Mit 36 ist ein Bauteil der erfindungsgemäßen Art bezeichnet, das an der Tür 3 der Kammer 1 befestigt ist und derart ausgebildet ist, dass eine Sichtverbindung zwischen den Stellflächen und der Türinnenfläche nicht besteht. Abgebogene Abschnitte 40 sorgen für die notwendige Überlappung der Abschirmbauteile im Bereich der vorderen Kanten des Stellplattenpaketes.With 36 a component of the type according to the invention is referred to, which is attached to the door 3 of the chamber 1 and is designed such that a visual connection between the shelves and the door inner surface does not exist. Bent portions 40 provide the necessary overlap of the shielding in the region of the front edges of the set of panels.
  • Die Abschirmbauteile sind temperiert. Sie sind als relativ dünne (weniger als 1 cm) doppelwandige Platten ausgebildet und von einem Heiz-/Kühlmedium (Sole) durchströmt. Zweckmäßig haben die Platten eine möglichst geringe Wärmekapazität und bestehen aus Edelstahl.The shielding components are tempered. They are designed as relatively thin (less than 1 cm) double-walled plates and flowed through by a heating / cooling medium (brine). Suitably, the plates have the lowest possible heat capacity and are made of stainless steel.
  • In Figur 1 ist ein vom Temperaturkreislauf 11 für die Stellplatten 4 unabhängiger Kreislauf 41 mit Wärmetauscher 42 und Heizung 43 dargestellt. Alle Abschirmbauteile sind Bestandteil dieses Kreislaufs 41. Über flexible Verbindungsleitungen 44 (Figur 2) ist auch das an der Kammertür 3 befestigte Bauteil 36 versorgt.FIG. 1 shows a circuit 41 with heat exchanger 42 and heating 43 which is independent of the temperature circuit 11 for the control panels 4. All shielding components are part of this circuit 41. Via flexible connecting lines 44 (Figure 2) and the attached to the chamber door 3 component 36 is supplied.
  • Es besteht zwar die Möglichkeit, die Abschirmbauteile auch in den Stellplattenkreislauf 11 einzubeziehen. Wegen der unterschiedlichen und-zeitlich versetzten Leistungsanforderungen sind jedoch zwei separate Kreisläufe 11 und 41 zweckmäßig. Der Steuerung des Kreislaufs 41 dient ebenfalls der Steuerblock 15.Although it is possible to include the Abschirmbauteile in the control plate circuit 11. However, because of the different and staggered power requirements, two separate circuits 11 and 41 are useful. The control of the circuit 41 is also the control block 15th
  • Die Figuren zeigen noch, dass sich der Drucksensor 16 im Raum 37 befindet. Als Steuergröße ist der Druck in diesem Raum 37 maßgebend. Der Druck au-ßerhalb des Raumes 37 ist für den gesteuerten Ablauf des Gefriertrocknungsprozesses unerheblich.The figures still show that the pressure sensor 16 is located in the space 37. The control variable is the pressure in this room 37. The pressure outside the space 37 is irrelevant to the controlled operation of the freeze-drying process.

Claims (8)

  1. Freeze-drying device with a chamber (1) comprising
    - a chamber wall (2) with interior wall surfaces,
    - temperature-controlled shelf plates (4) within the chamber (1), said shelf plates intended for arranging the vessels (5) containing the product to be freeze-dried,
    - a condenser (23) connected to the chamber (1) which serves to precipitate the water vapor that is brought forth during freeze-drying, as well as
    - temperature-controlled plate-shaped components (31 through 36) positioned between the shelf plates (4) and the interior wall surface of the chamber wall (2), said plate-shaped components forming an inner compartment (37) that surrounds the shelf plates (4);
    characterized by:
    the clearance between the components (31 through 36) forming the inner compartment (37) being such that the water vapor brought forth from the vessels (5) during freeze-drying can flow, essentially, unhindered through the spaces between the components (32 through 36) to the condenser (23), and the components (31 through 36) being positioned between the shelves (4) and the interior wall surfaces of chamber wall (2) such that they surround the shelves in such a way that there is no free line-of-sight from the shelf plates (4) and vessels (5) positioned thereon to the interior wall surfaces of the chamber wall (2).
  2. A chamber in accordance with claim 1, characterized by:
    the temperature-controlled components (31 through 36) being constructed of double-walled plates that are component parts of the cryogenic circuit (11, 41).
  3. A chamber in accordance with claim 1 or 2, characterized by:
    most of the temperature-controlled components or plates (31 through 36) being arranged to overlap each other such that optical impermeability is achieved.
  4. A chamber in accordance with claim 1, 2 or 3, characterized by:
    the temperature-controlled components or plates (31 through 36) being provided with bent sections (38, 39, 40) in order to achieve the optical impermeability, said bent sections enveloping the package of shelf plates on the sides, on the top and on the bottom.
  5. A chamber in accordance with anyone of the previous claims, characterized by:
    both the shelf plates (4) and the optical shield of temperature-controlled plates (31 through 36) being part of a mutual cryogenic circuit (11).
  6. A chamber in accordance with anyone of claims 1 through 4, characterized by:
    the shelf plates (4) and the optical shield of temperature-controlled plates (31 through 36) being part of individual cryogenic circuits (11, 41) that are independent of each other.
  7. A chamber in accordance with anyone of the previous claims with a chamber door, characterized by:
    its interior wall (36) carrying one or more of the temperature-controlled components or plates (31 through 36).
  8. A chamber in accordance with anyone of the previous claims, characterized by:
    a pressure sensor (16) being arranged within the optically impermeable space (37), and said pressure sensor being used to control the freeze-drying process.
EP20020791452 2001-07-27 2002-07-15 Chamber for a freeze-drying device Expired - Fee Related EP1412686B8 (en)

Priority Applications (3)

Application Number Priority Date Filing Date Title
DE10136498 2001-07-27
DE2001136498 DE10136498A1 (en) 2001-07-27 2001-07-27 Chamber for a freeze dryer
PCT/EP2002/007828 WO2003012355A1 (en) 2001-07-27 2002-07-15 Chamber for a freeze-drying device

Publications (3)

Publication Number Publication Date
EP1412686A1 EP1412686A1 (en) 2004-04-28
EP1412686B1 true EP1412686B1 (en) 2007-03-21
EP1412686B8 EP1412686B8 (en) 2007-05-09

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Application Number Title Priority Date Filing Date
EP01124001A Withdrawn EP1279913A1 (en) 2001-07-27 2001-10-09 Chamber for freeze drying apparatus
EP20020791452 Expired - Fee Related EP1412686B8 (en) 2001-07-27 2002-07-15 Chamber for a freeze-drying device

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Application Number Title Priority Date Filing Date
EP01124001A Withdrawn EP1279913A1 (en) 2001-07-27 2001-10-09 Chamber for freeze drying apparatus

Country Status (10)

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US (1) US6920701B2 (en)
EP (2) EP1279913A1 (en)
JP (1) JP3984591B2 (en)
AT (1) AT357638T (en)
AU (1) AU2002333243B2 (en)
DE (2) DE10136498A1 (en)
DK (1) DK1412686T3 (en)
ES (1) ES2284957T3 (en)
PT (1) PT1412686E (en)
WO (1) WO2003012355A1 (en)

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EP3070425A1 (en) 2015-03-16 2016-09-21 Martin Christ Gefriertrocknungsanlagen GmbH Freeze dryer having a viewing window

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DE10218007A1 (en) * 2002-04-23 2003-11-06 Bayer Ag Freeze dryer
DE102004007526A1 (en) * 2004-02-17 2005-09-01 Oetjen, Georg-Wilhelm, Dr. Method and device for the freeze-drying of products
WO2008057001A1 (en) * 2006-11-07 2008-05-15 Lev Kuzmich Kovalev Device for dehydrating materials in vacuum at a low-temperature
DE102007049278B4 (en) 2007-10-12 2010-08-05 Gea Lyophil Gmbh Devices for freeze-drying
US8371039B2 (en) * 2009-12-30 2013-02-12 Baxter International Inc. Thermal shielding to optimize lyophilization process for pre-filled syringes or vials
US8966782B2 (en) * 2010-09-28 2015-03-03 Baxter International Inc. Optimization of nucleation and crystallization for lyophilization using gap freezing
CN103140731B (en) 2010-09-28 2015-12-16 巴克斯特国际公司 Use freezing nucleation and the crystallization optimizing freeze-drying in gap
MX360701B (en) 2012-05-03 2018-11-14 Schott Ag Method and device for treating containers and substances stored therein for medical, pharmaceutical or cosmetic applications.
US9180145B2 (en) * 2012-10-12 2015-11-10 Mimedx Group, Inc. Compositions and methods for recruiting and localizing stem cells
US10480855B2 (en) * 2014-10-08 2019-11-19 Robert M. Parker Heated shelf for a freeze-drying system having a leading folded edge that does not catch on food being removed from the system
CN105004144B (en) * 2015-07-17 2017-03-29 上海化工研究院 A kind of superposition formula vacuum drying insulating box of variable volume
US10605527B2 (en) * 2015-09-22 2020-03-31 Millrock Technology, Inc. Apparatus and method for developing freeze drying protocols using small batches of product
US10676797B1 (en) * 2019-01-27 2020-06-09 Vinamit Usa Llc Concentrated sugarcane juice powder and method for preparing the same using the convection current freeze drying apparatus
US10966439B2 (en) * 2019-01-27 2021-04-06 Vinamit Usa Llc Concentrated fruit juice powder and method for preparing the same using a non-linear screw press juicer and convection current freeze drying apparatus
US10921058B2 (en) * 2019-01-27 2021-02-16 Vinamit Usa Llc Fully automatic convection current vacuum freeze drying method
US10451346B1 (en) * 2019-03-31 2019-10-22 Vinamit Usa Llc Convection current freeze drying apparatus and method of operating the same

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Publication number Priority date Publication date Assignee Title
EP3070425A1 (en) 2015-03-16 2016-09-21 Martin Christ Gefriertrocknungsanlagen GmbH Freeze dryer having a viewing window

Also Published As

Publication number Publication date
PT1412686E (en) 2007-06-29
EP1412686A1 (en) 2004-04-28
AT357638T (en) 2007-04-15
JP2004537025A (en) 2004-12-09
JP3984591B2 (en) 2007-10-03
US20040250441A1 (en) 2004-12-16
DE50209781D1 (en) 2007-05-03
DE10136498A1 (en) 2003-02-06
DK1412686T3 (en) 2007-07-30
WO2003012355A1 (en) 2003-02-13
US6920701B2 (en) 2005-07-26
EP1412686B8 (en) 2007-05-09
ES2284957T3 (en) 2007-11-16
AU2002333243B2 (en) 2007-05-24
EP1279913A1 (en) 2003-01-29

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