EP1279913A1 - Kammer für eine Gefriertrocknungseinrichtung - Google Patents

Kammer für eine Gefriertrocknungseinrichtung Download PDF

Info

Publication number
EP1279913A1
EP1279913A1 EP01124001A EP01124001A EP1279913A1 EP 1279913 A1 EP1279913 A1 EP 1279913A1 EP 01124001 A EP01124001 A EP 01124001A EP 01124001 A EP01124001 A EP 01124001A EP 1279913 A1 EP1279913 A1 EP 1279913A1
Authority
EP
European Patent Office
Prior art keywords
chamber
temperature
plates
chamber according
freeze
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.)
Withdrawn
Application number
EP01124001A
Other languages
German (de)
English (en)
French (fr)
Inventor
Peter Haseley
Georg-Wilhelm Dr. Oetjen
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
Steris 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 Steris GmbH filed Critical Steris GmbH
Publication of EP1279913A1 publication Critical patent/EP1279913A1/de
Withdrawn legal-status Critical Current

Links

Images

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 chamber for a freeze-drying device with temperature-adjustable shelves for containers in which the product to be freeze-dried is located.
  • Freeze drying has become particularly popular in the pharmaceutical industry for the preservation of medicines, vaccines, etc.
  • the chambers of modern freeze-drying facilities there is a plurality of shelves, on the shelves of which there are a large number of containers, vials or the like. (100,000 and more) finds space.
  • the product usually dissolved in water is filled into containers of this type.
  • the liquid is frozen. This step usually already takes place in the chamber of the freeze-drying device by cooling the shelves accordingly deep (-40 ° C to -60 ° C).
  • a chamber of the type mentioned at the outset is known from German Offenlegungsschrift 197 19 298. This document also explains a method for controlling the freeze drying process in the chamber.
  • the drying process is essentially characterized by two drying phases. As long as crystallized (frozen) water is still 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 by the dry product and more or less firmly bound. This water is removed during post-drying or desorption drying.
  • certain chamber pressures and shelf temperatures are used set. An essential parameter is the ice temperature, which can be determined by measuring the pressure rise.
  • Controlling the ice temperature in the sublimation area via the pressure presupposes that there is a uniform water vapor partial pressure in the chamber.
  • This uniform pressure distribution is only possible to a limited extent in the area of the chamber walls and chamber doors or doors.
  • the temperature of the product in the vial not only depends on the shelf temperature; the temperature of the inner walls of the chamber also affects heat radiation.
  • the water vapor emerging from the product has a temperature of -40 ° C
  • this temperature increases on the setting plates e.g. to -20 ° C, while the water vapor near the walls e.g. Reached 20 ° C. Due to these temperature differences, pressure differences of more than 10% can occur.
  • the desired requirement that there is a uniform water vapor partial pressure in the chamber is no longer met with sufficient accuracy; the ice temperature is no longer uniform. The result is a loss of product quality.
  • 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 to -60 ° C during freezing, which either leads to an impermissibly long freezing time or to separate cooling systems that have to give up several times more cooling capacity than required for the shelves 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, for example, -50 ° C.
  • the seals between the chamber and the door must remain functional at low temperatures and it is difficult to avoid condensation of the water vapor on these flanges.
  • a conceivable insulation of the flanges against water vapor condensation is technically not possible, since the 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.
  • the object of the present invention is to design a chamber for a freeze-drying device of the type mentioned at the outset without any particular technical outlay in such a way that uniform temperature and water vapor pressure ratios are established during the freeze-drying process.
  • this object is achieved in that an optical shield consisting of temperature-controlled components is provided between the shelves and the chamber inner surfaces. While the freeze-drying process is being carried out, the temperature-controlled components are each set to the temperature that the setting plates also have.
  • the chamber wall temperatures can no longer influence the temperature of the product in the vial. In the interior limited by the shielding components, there are no longer measurable differences in temperature and water vapor pressure.
  • the chamber is denoted by 1, the chamber wall by 2, its door by 3 (FIG. 2), the shelf plates located in chamber 1 by 4 and an example of a vial depicted on the shelf of a shelf plate 4 by 5.
  • the lower positioning plate 4 is supported on a stationary base plate 6.
  • the remaining setting plates 4 can be moved up and down (double arrow 7) in such a way that their distance changes.
  • a hydraulic drive pron rod 8
  • the vials 5 are closed in a known manner with stoppers which have laterally ending passage channels for the water vapor and are placed on the vials 5 before the start of the freeze-drying process.
  • the top plate 4 is attached to the plunger 9 of the piston rod 8.
  • the setting plates 4 are part of a temperature control circuit 11 indicated by dashed lines.
  • a brine flows through them, which, depending on requirements, is cooled in a heat exchanger 12 (connected to a refrigeration machine (not shown)) or heated with a heater 13.
  • the controlled sequence of the freeze-drying process is served by a control 15 shown as a block, to which signals from a pressure sensor 16 arranged in the chamber are supplied as a control variable.
  • the shelves are first cooled (freeze phase). During the Drying phases have temperatures above 0 ° C in order to accelerate the evaporation process.
  • the chamber 1 is equipped with a connecting piece 21 to which a condenser 23 and a vacuum pump 24 are connected via a valve 22.
  • the condenser 23 serves for the accumulation of the water vapor which is obtained during the freeze drying. Non-condensable gases are removed from the vacuum pump 24.
  • the valve 22 is connected to the controller 15. It is temporarily closed in order to be able to determine the ice temperature using pressure rise measurements.
  • a shield is provided between the shelves and the inner surfaces of the chamber wall 2. It consists of a number of components 31 to 36, which encompass the setting plates 4 in such a way that there is no line of sight between the setting areas and the bottles 5 placed thereon on the one hand and the chamber inner wall areas on the other.
  • the distances selected between the components are dimensioned so large that the water vapor transport between the shelves and the connecting piece 21 can take place essentially unhindered. It is therefore expedient if the individual components overlap like a blind.
  • the components 31 to 36 comprise the set of plates from all sides. Up and down, the upper and lower setting plate 4 form the desired, temperature-controlled privacy screen. If, for example, an upper positioning plate 4 is not present, one or more additional components must be present which provide the optical shielding towards the upper chamber wall.
  • the components according to the invention result in an inner, optically sealed space 37 in which the setting plates 4 or setting surfaces for the vials 5 are located. Radiant heat emanating from the chamber inner wall surfaces can no longer influence the temperature and pressure conditions in room 37. During the course of the freeze-drying process, the desired pressures and temperatures in room 37 are set uniformly.
  • the components 31, 32 have end sections bent at the top and bottom.
  • An alternative to this is shown in FIG. 2.
  • the components 31, 33 and 32, 33 each end with a gap that does not hinder the passage of steam in the area of the rear edges of the set of set plates.
  • Additional components 34, 35 are assigned to the columns at a sufficient distance, the width and length of which are selected such that there is no line of sight between the shelves and the chamber inner wall through the column.
  • Bent sections 40 ensure the necessary overlap of the shielding components in the region of the front edges of the set plate assembly.
  • the shielding components are tempered. They are designed as relatively thin (less than 1 cm) double-walled plates and a heating / cooling medium (brine) flows through them.
  • the plates expediently have the lowest possible heat capacity and are made of stainless steel.
  • FIG. 1 shows a circuit 41 with a heat exchanger 42 and heating 43 which is independent of the temperature circuit 11 for the setting plates 4. All shielding components are part of this circuit 41.
  • the component 36 fastened to the chamber door 3 is also supplied via flexible connecting lines 44 (FIG. 2).
  • the control block 15 also serves to control the circuit 41.
  • the figures also show that the pressure sensor 16 is in the room 37.
  • the pressure in this space 37 is decisive as the control variable.
  • the pressure outside the space 37 is irrelevant for the controlled sequence of the freeze-drying process.

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)
  • Vending Machines For Individual Products (AREA)
  • Physical Deposition Of Substances That Are Components Of Semiconductor Devices (AREA)
EP01124001A 2001-07-27 2001-10-09 Kammer für eine Gefriertrocknungseinrichtung Withdrawn EP1279913A1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE10136498A DE10136498A1 (de) 2001-07-27 2001-07-27 Kammer für eine Gefriertrocknungseinrichtung
DE10136498 2001-07-27

Publications (1)

Publication Number Publication Date
EP1279913A1 true EP1279913A1 (de) 2003-01-29

Family

ID=7693223

Family Applications (2)

Application Number Title Priority Date Filing Date
EP01124001A Withdrawn EP1279913A1 (de) 2001-07-27 2001-10-09 Kammer für eine Gefriertrocknungseinrichtung
EP02791452A Expired - Lifetime EP1412686B8 (de) 2001-07-27 2002-07-15 Kammer für eine gefriertrocknungseinrichtung

Family Applications After (1)

Application Number Title Priority Date Filing Date
EP02791452A Expired - Lifetime EP1412686B8 (de) 2001-07-27 2002-07-15 Kammer für eine gefriertrocknungseinrichtung

Country Status (10)

Country Link
US (1) US6920701B2 (ja)
EP (2) EP1279913A1 (ja)
JP (1) JP3984591B2 (ja)
AT (1) ATE357638T1 (ja)
AU (1) AU2002333243B2 (ja)
DE (2) DE10136498A1 (ja)
DK (1) DK1412686T3 (ja)
ES (1) ES2284957T3 (ja)
PT (1) PT1412686E (ja)
WO (1) WO2003012355A1 (ja)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2003091645A1 (de) * 2002-04-23 2003-11-06 Bayer Technology Services Gmbh Gefriertrockenvorrichtung
CN105004144A (zh) * 2015-07-17 2015-10-28 上海化工研究院 一种可变容积的迭加式真空干燥恒温箱
EP3070425A1 (de) * 2015-03-16 2016-09-21 Martin Christ Gefriertrocknungsanlagen GmbH Gefriertrockner mit einem Sichtfenster
US20200240706A1 (en) * 2019-01-27 2020-07-30 Vinamit Usa Llc Fully automatic convection current vacuum freeze drying method

Families Citing this family (19)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102004007526A1 (de) * 2004-02-17 2005-09-01 Oetjen, Georg-Wilhelm, Dr. Verfahren und Einrichtung zur Gefriertrocknung von Produkten
WO2008057001A1 (fr) * 2006-11-07 2008-05-15 Lev Kuzmich Kovalev Dispositif de déshydratation à basse température de matériaux sous vide
DE102007049278B4 (de) 2007-10-12 2010-08-05 Gea Lyophil Gmbh Vorrichtungen zum Gefriertrocknen
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
US8689460B2 (en) 2010-09-28 2014-04-08 Baxter International Inc. Optimization of nucleation and crystallization for lyophilization using gap freezing
KR20150009982A (ko) 2012-05-03 2015-01-27 쇼오트 아게 의료, 제약 또는 화장품 어플리케이션들을 위한 물질들을 저장하기 위한 컨테이너들을 처리하기 위한 방법 및 장치
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
US10605527B2 (en) 2015-09-22 2020-03-31 Millrock Technology, Inc. Apparatus and method for developing freeze drying protocols using small batches of product
EP3392584B1 (en) * 2017-04-21 2019-12-18 GEA Lyophil GmbH A freeze dryer and a method for inducing nucleation in products
US10451346B1 (en) * 2019-03-31 2019-10-22 Vinamit Usa Llc Convection current freeze drying apparatus and method of operating the same
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
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
JP7390176B2 (ja) * 2019-12-06 2023-12-01 株式会社アルバック 真空乾燥装置、真空乾燥装置における棚の温度調節方法
JP2021096030A (ja) * 2019-12-17 2021-06-24 株式会社アルバック 真空乾燥装置、真空乾燥装置における棚の温度調節方法
US11054185B1 (en) * 2020-02-24 2021-07-06 Lyophilization Technology, Inc. Apparatus for lyophilization of products contained in product delivery units
US11506455B2 (en) * 2020-03-05 2022-11-22 Green Mountain Mechanical Design, Inc. Partial vacuum drying system and method
CN116045606B (zh) * 2023-01-13 2023-09-22 浙江毓昌生物技术有限公司 一种冷冻箱及操作方法

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3048928A (en) * 1959-04-27 1962-08-14 Raytheon Co Freeze-drying apparatus
GB1032857A (en) * 1962-04-09 1966-06-15 Cryo Maid Improved method and apparatus for producing readily reconstitutable food products byfreeze drying
US3311991A (en) * 1965-04-20 1967-04-04 Pillsbury Co Drying apparatus and method
WO1997008503A1 (fr) * 1995-08-22 1997-03-06 Laboratoire Français Du Fractionnement Et Des Biotechnologies Emballage etanche pour sechage, notamment lyophilisation, et procede de sechage, notamment de lyophilisation, a l'aide d'un tel emballage
DE19719398A1 (de) 1997-05-07 1998-11-12 Amsco Finn Aqua Gmbh Verfahren zur Steuerung eines Gefriertrocknungsprozesses

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3762065A (en) * 1971-04-12 1973-10-02 Kamas Kvarnmaskiner Ab Apparatus for drying materials
WO1996022496A1 (en) * 1995-01-20 1996-07-25 Freezedry Specialties, Inc. Freeze dryer
GB9505523D0 (en) * 1995-03-18 1995-05-03 Wellcome Found Lyophilization process
AT1399U1 (de) * 1995-11-29 1997-04-25 Immuno Ag Verfahren und einrichtung zum lyophilisieren

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3048928A (en) * 1959-04-27 1962-08-14 Raytheon Co Freeze-drying apparatus
GB1032857A (en) * 1962-04-09 1966-06-15 Cryo Maid Improved method and apparatus for producing readily reconstitutable food products byfreeze drying
US3311991A (en) * 1965-04-20 1967-04-04 Pillsbury Co Drying apparatus and method
WO1997008503A1 (fr) * 1995-08-22 1997-03-06 Laboratoire Français Du Fractionnement Et Des Biotechnologies Emballage etanche pour sechage, notamment lyophilisation, et procede de sechage, notamment de lyophilisation, a l'aide d'un tel emballage
DE19719398A1 (de) 1997-05-07 1998-11-12 Amsco Finn Aqua Gmbh Verfahren zur Steuerung eines Gefriertrocknungsprozesses

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2003091645A1 (de) * 2002-04-23 2003-11-06 Bayer Technology Services Gmbh Gefriertrockenvorrichtung
US6931754B2 (en) 2002-04-23 2005-08-23 Bayer Aktiengesellschaft Freeze-drying apparatus
EP3070425A1 (de) * 2015-03-16 2016-09-21 Martin Christ Gefriertrocknungsanlagen GmbH Gefriertrockner mit einem Sichtfenster
CN105004144A (zh) * 2015-07-17 2015-10-28 上海化工研究院 一种可变容积的迭加式真空干燥恒温箱
US20200240706A1 (en) * 2019-01-27 2020-07-30 Vinamit Usa Llc Fully automatic convection current vacuum freeze drying method
US10921058B2 (en) * 2019-01-27 2021-02-16 Vinamit Usa Llc Fully automatic convection current vacuum freeze drying method

Also Published As

Publication number Publication date
WO2003012355A1 (de) 2003-02-13
AU2002333243B2 (en) 2007-05-24
EP1412686B1 (de) 2007-03-21
ATE357638T1 (de) 2007-04-15
US20040250441A1 (en) 2004-12-16
EP1412686B8 (de) 2007-05-09
EP1412686A1 (de) 2004-04-28
DE10136498A1 (de) 2003-02-06
DE50209781D1 (de) 2007-05-03
PT1412686E (pt) 2007-06-29
ES2284957T3 (es) 2007-11-16
JP3984591B2 (ja) 2007-10-03
DK1412686T3 (da) 2007-07-30
US6920701B2 (en) 2005-07-26
JP2004537025A (ja) 2004-12-09

Similar Documents

Publication Publication Date Title
EP1412686B1 (de) Kammer für eine gefriertrocknungseinrichtung
EP1354028B1 (de) Klimatisierter lagerschrank
EP0980503B1 (de) Verfahren und vorrichtung zur steuerung eines gefriertrocknungsprozesses
EP1502063B1 (de) Gefriertrockenvorrichtung
DE3621562A1 (de) Kaeltemaschine
DE10010718B4 (de) Aufbewahr- und Transportbehälter für leicht verderbliche Produkte
EP2354729B1 (de) Vorrichtung zur Einstellung tiefkalter Temperaturen
WO2010034043A1 (de) Plattenfallfilm-kurzweg verdampfer
EP0278039B1 (de) Einrichtung zur Gefriertrocknung
DE102007049278B4 (de) Vorrichtungen zum Gefriertrocknen
EP0136458A1 (de) Behälter zum Kühlen eines Kühlgutes
DE4000913A1 (de) Verfahren und vorrichtung zum einfrieren eines der gefriertrocknung zu unterwerfenden produktes
EP0864071A1 (de) Verfahren und einrichtung zum lyophilisieren sowie behälter und füllanlage
CH694924A5 (de) Weinlagerschrank.
DE29611521U1 (de) Vorrichtung zum Trocknen von Holz
EP1437073B1 (de) Kühlmöbel als Zusatz für zwei Kühltruhen
DE1102653B (de) Vakuumgefrierkammertrockner
DE2235483C3 (de) Vorrichtung zum Gefriertrocknen von in geringen Mengen in Behältern zu trocknendem Gut
EP0330890A2 (de) Anlage zur Sublimationstrocknung von Stoffen
DE1243705B (de) Kuehlschrank
DE9320092U1 (de) Kühlvorrichtung zur Langzeit-Lagerung von gefrorenen Blutprodukten
DE926912C (de) Kuehlschrank, insbesondere fuer Haushaltungen
DE2129715B2 (de) Kühlung von in warmem Zustand abgefüllten Produkten
EP0608699A2 (de) Kühlgerät
DE15840C (de) Trockenverfahren für Raffinade

Legal Events

Date Code Title Description
PUAI Public reference made under article 153(3) epc to a published international application that has entered the european phase

Free format text: ORIGINAL CODE: 0009012

AK Designated contracting states

Designated state(s): AT BE CH CY DE DK ES FI FR GB GR IE IT LI LU MC NL PT SE TR

AX Request for extension of the european patent

Extension state: AL LT LV MK RO SI

AKX Designation fees paid

Designated state(s): AT BE CH CY DE DK ES FI FR GB GR IE IT LI LU MC NL PT SE TR

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: THE APPLICATION IS DEEMED TO BE WITHDRAWN

18D Application deemed to be withdrawn

Effective date: 20030730