EP0278039B1 - Einrichtung zur Gefriertrocknung - Google Patents

Einrichtung zur Gefriertrocknung Download PDF

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Publication number
EP0278039B1
EP0278039B1 EP87102062A EP87102062A EP0278039B1 EP 0278039 B1 EP0278039 B1 EP 0278039B1 EP 87102062 A EP87102062 A EP 87102062A EP 87102062 A EP87102062 A EP 87102062A EP 0278039 B1 EP0278039 B1 EP 0278039B1
Authority
EP
European Patent Office
Prior art keywords
chamber
freeze
piston rod
drying
sterilization
Prior art date
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.)
Expired - Lifetime
Application number
EP87102062A
Other languages
German (de)
English (en)
French (fr)
Other versions
EP0278039A1 (de
Inventor
Heinz May
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
Finn Aqua Santasalo Sohlberg 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 Finn Aqua Santasalo Sohlberg GmbH filed Critical Finn Aqua Santasalo Sohlberg GmbH
Priority to ES198787102062T priority Critical patent/ES2028804T3/es
Priority to DE8787102062T priority patent/DE3775205D1/de
Priority to EP87102062A priority patent/EP0278039B1/de
Priority to JP63024118A priority patent/JP2652185B2/ja
Priority to DK071988A priority patent/DK71988A/da
Priority to US07/156,002 priority patent/US4881326A/en
Publication of EP0278039A1 publication Critical patent/EP0278039A1/de
Application granted granted Critical
Publication of EP0278039B1 publication Critical patent/EP0278039B1/de
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • 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 device for freeze-drying products located in containers (bottles, vials) with a chamber, a plurality of adjusting plates arranged vertically displaceably in the chamber and with at least one piston rod serving to displace the adjusting plates, the actuating device of which is arranged outside the chamber.
  • 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 proceeds approximately as follows: During a first phase, the water-containing product is frozen (for example at a shelf temperature of -40 ° C). Then the sublimation of the water in ice form takes place, under vacuum (about 10 ⁇ 1 mbar). After this main drying, the post-drying takes place in order to achieve extremely low residual moisture. The product is heated as much as possible during the final drying. The pressure at which post-drying takes place is around 10 ⁇ 3 mbar.
  • freeze-drying chamber Only after a sterilization process of this type is the freeze-drying chamber loaded with the containers in which the product to be lyophilized is located. These have also been prepared sterile. Loading is also carried out from a sterile room.
  • the piston rod is retracted during the loading process or following the freeze-drying process in order to change the height of the setting plates or to close the containers, a non-sterile section of the piston rod then enters the Chamber that can still be under a pressure of 10 von3 mbar after a freeze-drying process, for example. During this time, there is a risk that undesirable contamination, particularly of the product, will take place.
  • the present invention has for its object to eliminate this risk of contamination in freeze-drying devices of the type mentioned.
  • the piston rod is assigned a chamber for sterilizing the piston rod section entering the freeze-drying chamber, that the sterilization chamber is cylindrical, that it surrounds the piston rod section entering the freeze-drying chamber to form an annular space, and that it has connections for one Vacuum pump and for the supply of sterilization or inert gases.
  • the sterilization chamber and so that the piston rod section therein is also sterilized in the manner described before the actual freeze-drying process or at another time, for example during the "freezing" process phase, then the piston rod section entering the freeze-drying chamber after the end of the freeze-drying process is sterile. There is no longer any risk of undesirable contamination during the adjustment of the shelf.
  • FIG. 1 the freeze drying chamber 1 and the height-adjustable shelves 2 located therein are shown only schematically.
  • the capacitor which is usually still present, has not been shown.
  • a cylinder-piston device (closure device) 4 which is only shown in part, is supported on the freeze-drying chamber 1 via a steel frame 3.
  • the not visible piston of this device 4 is connected to a piston rod 5, the free end of which projects from above into the freeze-drying chamber 1 and carries a pressure plate 6.
  • a lowering of the piston and thus the piston rod 5 causes the setting plates 2 to move together.
  • This process forms, for example, the end of a freeze-drying process for products which are located in containers (bottles, vials) with special stoppers placed on the setting plates 2.
  • the moving together of the setting plates 2 causes the plugs to be pressed into the containers and thus to close the containers. This enables the containers to be sealed under vacuum or an inert gas atmosphere.
  • the piston rod 5 is assigned a separate sterilization chamber 7.
  • This consists of the cylindrical tube 8, which surrounds the piston rod 5 to form the annular space 9.
  • the end of the annular chamber 9 is formed by flanges 11 and 12, which are each sealed off from the piston rod by means of a double seal 13, 14.
  • the distance from the seal 11, 13 located in the area of the closure device 4 to the chamber-side seal 12, 14 is selected so that the section of the piston rod 5 which maximally enters the chamber 1 is accommodated therein.
  • the chamber-side seal 12, 14 is shown enlarged again in FIG. 2.
  • the cylindrical wall of the chamber 9 is equipped with two connections 15 and 16, to which the devices used to carry out the sterilization are connected.
  • the connection of steam (valve 17), the removal of steam (valve 18) and the supply of sterile air or sterile inert gas (valve 19) take place via the connection 15.
  • a water ring pump 21 (via the valve 22) and a rotary vane pump 23 (via the valve 24) are connected to the connection 16.
  • the control 25, shown schematically as a block, is provided. This is connected to a temperature sensor 26 and to a pressure sensor 27, which are connected to the cylindrical wall 8 of the chamber 9 and supply electrical signals corresponding to the temperature or pressure within the chamber 9. Depending on these signals and the desired steam exposure time, the sterilization process described above takes place automatically. This can be done at any time, regardless of or simultaneously with the sterilization of the other parts of the system. However, all facilities that are suitable for Sterilization of the piston rod 5 and the freeze drying system itself are required only once and are used in a targeted manner via control means.
  • the tubular section 31 of the flange 12 is surrounded by two annular fittings 36 and 37 with radial bores 38 and 39.
  • the adapter 36 is welded to the wall of the chamber 1 and sealed both to the flange 12 and to the adapter 37 with sealing rings 41, 42.
  • the radial bore 38 is concentric with a radial bore 43 in the flange 12. This creates a channel through which the piston rod section located between the sealing rings 32 and 33 is accessible.
  • the bore 42 opens into an annular channel 45 which surrounds the piston rod 5. This makes it possible to supply superheated steam to this area of the seal during the course of the sterilization process, so that effective sterilization also takes place in the area of the double seal 14. This effort could be dispensed with if the piston rod 5 were to travel the distance, for example back and forth, during the sterilization, which corresponds to the height of the chamber-side seal 12, 14.
  • the fitting 37 is welded to the cylindrical wall 8 of the chamber 9 and forms with the tubular portion 31 of the flange 12 an annular space 44 which the Radial bore 39 connects to the sterilization chamber 9. Condensate is drawn off via the annular space 44 and the channel 39 during the course of the sterilization process.
  • the piston rod is arranged above the freeze-drying chamber 1. It is therefore expedient for the chamber-side seal 12, 14 to be carefully sterilized by the measures shown in FIG. 2 and for the condensate which is formed to be drawn off in this area too. If the piston rod is pushed into the freeze-drying chamber 1 from below in a manner known per se, then the measures for removing the condensate must be provided in the area of the lower seal, that is to say in the area of the seal adjacent to the cylinder-piston device.

Landscapes

  • Engineering & Computer Science (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Molecular Biology (AREA)
  • Mechanical Engineering (AREA)
  • General Engineering & Computer Science (AREA)
  • Drying Of Solid Materials (AREA)
EP87102062A 1987-02-13 1987-02-13 Einrichtung zur Gefriertrocknung Expired - Lifetime EP0278039B1 (de)

Priority Applications (6)

Application Number Priority Date Filing Date Title
ES198787102062T ES2028804T3 (es) 1987-02-13 1987-02-13 Instalacion para la liofilizacion.
DE8787102062T DE3775205D1 (de) 1987-02-13 1987-02-13 Einrichtung zur gefriertrocknung.
EP87102062A EP0278039B1 (de) 1987-02-13 1987-02-13 Einrichtung zur Gefriertrocknung
JP63024118A JP2652185B2 (ja) 1987-02-13 1988-02-05 凍結乾燥装置
DK071988A DK71988A (da) 1987-02-13 1988-02-12 Frysetoerreapparat
US07/156,002 US4881326A (en) 1987-02-13 1988-02-16 Sterilizing device for a freeze-drying apparatus

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
EP87102062A EP0278039B1 (de) 1987-02-13 1987-02-13 Einrichtung zur Gefriertrocknung

Publications (2)

Publication Number Publication Date
EP0278039A1 EP0278039A1 (de) 1988-08-17
EP0278039B1 true EP0278039B1 (de) 1991-12-11

Family

ID=8196753

Family Applications (1)

Application Number Title Priority Date Filing Date
EP87102062A Expired - Lifetime EP0278039B1 (de) 1987-02-13 1987-02-13 Einrichtung zur Gefriertrocknung

Country Status (6)

Country Link
US (1) US4881326A (da)
EP (1) EP0278039B1 (da)
JP (1) JP2652185B2 (da)
DE (1) DE3775205D1 (da)
DK (1) DK71988A (da)
ES (1) ES2028804T3 (da)

Families Citing this family (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5288460A (en) * 1989-03-08 1994-02-22 Abtox, Inc. Plasma cycling sterilizing process
FR2655020B1 (fr) * 1989-11-30 1992-03-27 Usifroid Mecanisme de bouchage de flacons dans une cuve de lyophilisation.
CA2146090C (en) * 1994-05-10 1998-11-24 Mark E. Mitchell Apparatus and method of mixing materials in a sterile environment
AT1399U1 (de) 1995-11-29 1997-04-25 Immuno Ag Verfahren und einrichtung zum lyophilisieren
US5701745A (en) * 1996-12-16 1997-12-30 Praxair Technology, Inc. Cryogenic cold shelf
JP3985241B2 (ja) * 1998-09-18 2007-10-03 株式会社アルバック 凍結真空乾燥装置
WO2004029529A1 (de) 2002-09-18 2004-04-08 Sueverkruep Richard Verfahren zum herstellen einer zubereitung eines pharmazeutischen materials als lyophilisat und anlage hierfür
DE102008017461B4 (de) 2008-04-03 2010-04-15 Süverkrüp, Richard, Prof. Dr. Vorrichtung und Verfahren zur Herstellung eines pulverförmigen lyophilisierten Materials, bestehend aus annähernd gleich großen kugelförmigen Teilchen
ATE520940T1 (de) * 2008-05-26 2011-09-15 Paolo Debolini Trockner, insbesondere für pulverisiertes oder granulatförmiges material
DK3004767T3 (da) 2013-05-29 2018-01-15 Gea Process Engineering As Steril frysetørring.

Family Cites Families (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2353986A (en) * 1938-11-07 1944-07-18 Sharp & Dohme Inc Preservation
GB701888A (en) * 1951-06-26 1954-01-06 Alois Vogt Improvements in or relating to processes and apparatus for freeze-drying
US3280471A (en) * 1964-11-23 1966-10-25 American Sterilizer Co Apparatus and process for freeze drying
US3448556A (en) * 1965-12-06 1969-06-10 Everett Ray Taggart Apparatus for preserving biological and like preparations
US3451189A (en) * 1967-04-14 1969-06-24 Everett R Taggart Desiccator apparatus including improved vacuum bottle capping arrangement
GB1423353A (en) * 1972-06-19 1976-02-04 Boc International Ltd Vacuum lock
JPS4930737A (da) * 1972-07-25 1974-03-19
DE2556467C2 (de) * 1975-12-15 1987-03-26 EKATO Industrieanlagen Verwaltungsgesellschaft mbH u. Co, 7860 Schopfheim Verfahren und Vorrichtung zur ständigen thermischen Sterilisation von Dichtungen
JPS52142360A (en) * 1976-04-22 1977-11-28 Kiyoshi Shimada Apparatus for changing space between shelves in freeze vacuum drying machine
JPS5570255A (en) * 1978-11-21 1980-05-27 Tomoe Shokai Kk Method of removing remaining medicine and its device

Also Published As

Publication number Publication date
DK71988D0 (da) 1988-02-12
US4881326A (en) 1989-11-21
JP2652185B2 (ja) 1997-09-10
DE3775205D1 (de) 1992-01-23
EP0278039A1 (de) 1988-08-17
JPS63207978A (ja) 1988-08-29
ES2028804T3 (es) 1992-07-16
DK71988A (da) 1988-08-14

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