EP1502063B1 - Dispositif de lyophilisation - Google Patents

Dispositif de lyophilisation Download PDF

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Publication number
EP1502063B1
EP1502063B1 EP03722477A EP03722477A EP1502063B1 EP 1502063 B1 EP1502063 B1 EP 1502063B1 EP 03722477 A EP03722477 A EP 03722477A EP 03722477 A EP03722477 A EP 03722477A EP 1502063 B1 EP1502063 B1 EP 1502063B1
Authority
EP
European Patent Office
Prior art keywords
heating
temperature
plates
chamber
cooling
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
EP03722477A
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German (de)
English (en)
Other versions
EP1502063A1 (fr
Inventor
Bernd Sennhenn
Dietrich Gehrmann
Ariane Firus
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.)
HOF-Sonderanlagenbau GmbH
Original Assignee
HOF-Sonderanlagenbau GmbH
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Filing date
Publication date
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Publication of EP1502063A1 publication Critical patent/EP1502063A1/fr
Application granted granted Critical
Publication of EP1502063B1 publication Critical patent/EP1502063B1/fr
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 freeze-drying chamber with coolable / heatable shelves for a variety of istgefiillten containers or assignable with product layers cool / heatable control panels with special facilities that eliminate the drying progress dependent harmful temperature influences the chamber wall surfaces.
  • Special versions allow the avoidance of high energy loss through a special chamber wall construction with simultaneous mass reduction of the tempered components
  • Driving potential for drying are temperature differences between product-filled containers or product layers and their environment, which provides the potential necessary for the progress of freeze-drying. This potential is greater in the edge region of the control panels than in the middle of the control panel, because direct heat exchange by radiation and convection takes place between containers at the edge and the chamber wall.
  • the natural convection of the gas in the free gap between wall and temperature-controlled control panels acts particularly strongly as a heat carrier for the convection current exposed container. These additional heat flows decrease towards the center of the plate and thus cause the inhomogeneous freezing and drying process of the containers or product layers distributed over the plate.
  • Freeze dryers are made according to the prior art either entirely without tempering the chamber walls or with heating /deinäntelt which are applied directly to the supporting structure.
  • These heating / cooling jackets have the purpose of the chamber to cool down from the sterilization temperature to the temperature suitable for loading because of the short to ground with the heavy supporting structure of the chamber. Thereafter, the coolant is usually emptied from these heating / cooling surfaces to reduce mass.
  • the cooling of the chamber wall to a temperature which eliminates the driving potential responsible for the disturbance is not possible with these constructions.
  • the invention relates to a drying apparatus for removing solvent from moist material, comprising at least one drying chamber with at least one adjusting plate for receiving wet-filled containers or layers of moist material, wherein the drying chamber is connected to a condenser via a vapor channel in which the sublimated solvent is separable, wherein the control panels are connected to a temperature-controlled heating / cooling circuit, the chamber having heating / cooling plates, which are connected to a second heat transfer circuit and wherein the Heating / cooling plates are carried out largely thermally decoupled from the chamber wall, characterized in that the heating / cooling plates are suspended parallel to the edges of the adjusting plates at a distance from the adjusting plates in the drying chamber, so that the hanging heating / cooling plates a nearly closed Form radiation cage around the stack of piles.
  • the elimination of the non-uniformity is achieved by controlled heating / cooling plates, which surround the control panels like a radiation cage, which are adjusted so that there is no driving temperature gradient between wall and container.
  • the resulting homogeneity of the freezing and drying process of all containers can improve the uniformity of the product quality and significantly increase the drying capacity.
  • control panels can be provided with a piping system.
  • the pipe system is traversed by a stream of temperature-controlled heat transfer medium, which is supplied from a heating / cooling system.
  • a preferred drying apparatus is characterized in that the heating / cooling plates are spaced from the chamber wall.
  • the outer chamber wall is pressure-resistant, so that the surface forces are absorbed without deformation during evacuation of the chamber.
  • drying apparatus wherein the outer chamber wall has thermal insulation to minimize energy loss of the system.
  • thermoforming apparatus in which the heating / cooling plates are vacuum-tightly connected to the chamber wall, so that effectively results in a 2-chamber system
  • the heating / cooling surfaces are mechanically connected in particular via spacers with the inside of the chamber wall and form with this an evacuated planar gap.
  • vacuum connections are provided in the chamber wall.
  • Preference is furthermore a drying apparatus, characterized in that the gap is adjustable by a vacuum system to the pressure level of the drying chamber for the purpose of pressure equalization.
  • the spacers are preferably made of poorly heat-conducting material, in particular stainless steel.
  • a particular embodiment of the drying apparatus is characterized in that elastic connecting plates between the side heating / cooling plates and the chamber wall are designed so flexible that the temperature-induced changes in length of the heating / cooling surfaces are compensated without material damage.
  • the drying chamber is already evacuated during the freezing process in order to reduce convection influences.
  • the chamber wall has a special design on an external heat insulation.
  • the CIP / SIP devices are mounted so that all surfaces can be cleaned.
  • a drying apparatus characterized in that the temperature control systems for the heating / cooling plates are sensor-controlled to the appropriate temperature adjustable.
  • the temperature control systems for the heating / cooling plates are predictively controlled by a computer program controlled to the appropriate temperature.
  • the temperature control systems for the heating / cooling plates are controlled by a hybrid system of sensor and computer and set to the appropriate temperature.
  • the inventive arrangement of the heating / cooling plates equal mass ratios between heating / cooling plates and control panels are made and thus allows approximately the same temperature / time profiles for walls and panels / container.
  • the regulation / control of the heating / cooling plate temperature can be carried out according to the following strategies:
  • Sensor-controlled control During the freezing phase, the control panels and heating / cooling plates are controlled following the same temperature program. After the start of the drying program, the heating / cooling plate temperature and the plate temperature follow different programs. The platen temperature is determined by the given Lyozyklus and it is traversed and regulated in the Lyozyklus specified temperature / Zeitprogamm. The temperature of the heating / cooling plates is set in the first drying section on the sublimation of the frozen product, which adjusts chamber pressure-dependent and solvent-dependent. As a first approximation, this temperature can be calculated on the basis of the material values. Measurements of the sublimation temperature in the laboratory experiment can be used to correct this calculated temperature. It is also possible to use the pressure rise method for the direct determination of the sublimation temperature, as described, for example, by GW Oetjen in "Gefriertrocknen", VCH Verlag, 1997.
  • the temperature of the heating / cooling plates must be changed when the second drying section starts.
  • the beginning of the second drying section can be detected by measuring the system pressure in the gas stream from the freezing chamber with different pressure measuring probes, eg: an absolute pressure gauge and a conductivity probe (eg Pirani probe) set to nitrogen. If the solvent vapor flow approaches 0 at the end of the first drying section, both measured values approach the same value, since the nitrogen content in the gas flow increases steadily and thus the measured value of the Pirani probe approaches more and more the absolute pressure measured value.
  • the temperature of the heating / cooling plates can now be slowly raised to the plate temperature and be tracked in the further course of drying the platen temperature. For example, the degree of approach to the platen temperature is determined as a function of the pressure difference between the two pressure readings.
  • Predictive control of the heating / cooling plates If, in the laboratory test, drying characteristics were recorded on the product to be dried under defined conditions and a drying program was used to determine all freeze drying properties / parameters of the product, the drying process can be determined with knowledge of the freeze drying properties of the freeze dryer of the product and the values of the product temperature determined by the calculation program are used as the reference variable for the heating / cooling plate temperatures. This method is in Fig. 3b shown.
  • Hybrid method From the measurements in the freeze dryer (absolute pressure, pressure according to conductivity probe) and simulation calculations, the product temperatures are determined and used as a reference variable for the heating / cooling plate temperature.
  • a conventional system of freeze-drying chamber 1 and condenser chamber 22 is shown in which packages of product-filled containers are frozen and freeze-dried.
  • Container 3 are indicated on the shelf 2 in the edge and middle area standing.
  • the chamber 1 has two separately openable doors 11, 11a, which are sealed.
  • the freeze-drying chamber 1 has a bivalve structure.
  • the heavy chamber wall construction 6 with reinforcing ribs 7 has the task of offering a vacuum-tight, torsionally stiff housing, which withstands atmospheric pressure during evacuation of the freeze-drying chamber 1, for the second, inner chamber 23 integrated therein.
  • the chamber 1 is equipped with thermal insulation material 8 on its outside against heat exchange with the environment.
  • the inner freeze-drying chamber 23 is formed from the heating / cooling plates 4, which are held by means of spacers 5 at a distance from the chamber wall 6, pressure-tight connected via flexible sheets 9 with the chamber wall 6, so that the gap 24 between heating / cooling plates and supporting wall 6 of the chamber 1 can be evacuated.
  • the evacuation takes place via pipelines 10, 12, which are connected to the main vacuum pump 21 via valves 20.
  • the evacuation of the gap 24 serves two purposes: First, the pressure equalization between freeze-drying chamber 23 and the space 24 between heating / cooling plates 4 and chamber wall 6, so that pressure forces on the heating / cooling plates 4 are avoided. Second, it serves to lower the heat exchanger by the pressure-dependent lowering of the effective heat conduction of the intermediate space 24.
  • the same pressure as in the freeze-drying chamber 23 p ⁇ 0.1 mbar
  • the gap 24 as the evacuated Gap of a Dewar flask acts.
  • the spacers 5 between the heating / cooling plates 4 and the chamber wall 6 are made of a poorly heat-conductive material (eg stainless steel), and the number of spacers 5 is minimized to the necessary extent, so that the heat transfer is minimized by heat conduction through the spacers 5 ,
  • the connecting plates 9 are structurally designed so that the temperature-dependent change in length of the heating / cooling plates 4 can be absorbed by the sheets without risk to the mechanical strength of the connection to the chamber wall 6. In this way, a smooth-surface freeze-drying chamber 23, which can be easily cleaned.
  • the heating / cooling plates 4 are supplied via a separately controllable temperature control (not shown) with heat transfer fluid (silicone oil), which is discharged via the line 13 and line 14.
  • the temperature control system uses the same heat transfer medium as the control panels and can be supplied from the same reservoir.
  • the temperature control system for the heating / cooling plates 4 must always be operated with a temperature adjusted to the vial temperature, while the heat transfer medium for the control plates 2 follows another temperature program following the Lyo cycle.
  • the temperature program for the heating / cooling plates 4 depends on the temperature of the container. This method is already described in general above.
  • FIG. 2 another embodiment of the freeze dryer with respect to the attachment of heating / cooling plates 4 'is shown.
  • the tempered plates 4 ' hang freely in the chamber 23.
  • the heating / cooling plates 4' are suspended parallel to the edges of the panels 2 at a distance, so that space for all the panels 2 associated organs eg tubes 25, 26 for the Heat transfer medium, shelf holder (not shown), is maintained.
  • Known CIP / SIP devices can also be provided in the chamber interior.
  • the heating / cooling plates 4 'are in turn fed by a separate heat transfer circuit via inlet 13 and return 14 with the heat transfer medium.
  • the crowd the heating / cooling plates corresponds in both cases (according to Example 1 and 2) of the mass of the adjusting plates 2, so that the heating / cooling dynamics of the plates 2 and 4 or 4 'are matched and no temperature shifts caused by mass inequality.

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  • 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)
  • Paper (AREA)
  • Seal Device For Vehicle (AREA)
  • Apparatus For Disinfection Or Sterilisation (AREA)

Claims (13)

  1. Appareil de séchage (1) destiné à l'élimination de solvant contenu dans une matière humide, consistant au moins en une chambre de séchage (23) avec au moins une plaque de positionnement (2) destinée à recevoir des récipients (3) remplis de matière humide ou avec des couches planes de matière humide, la chambre de séchage (23) étant reliée à un condenseur (22) par l'intermédiaire d'un canal de vapeur (15) dans lequel le solvant sublimé peut se précipiter, les plaques de positionnement (2) étant reliées à un premier circuit de chauffage/de refroidissement régulé en température, la chambre (23) comportant des plaques de chauffage/de refroidissement (4) ou (4') qui sont reliées à un deuxième circuit caloporteur, les plaques de chauffage/de refroidissement (4) ou (4') étant réalisées de manière à être en grande partie thermiquement découplées de la paroi (6) de la chambre,
    caractérisé en ce
    que les plaques de chauffage/de refroidissement (4') sont suspendues parallèlement aux bords des plaques de positionnement (2) à distance des plaques de positionnement (2) dans la chambre de séchage (1) de sorte que les plaques de chauffage/de refroidissement (4') suspendues forment une cage de radiation presque fermée autour de la pile de plaques de positionnement.
  2. Appareil de séchage selon la revendication 1,
    caractérisé en ce
    que les plaques de chauffage/de refroidissement (4) ou (4') sont disposées à distance de la paroi (6) de la chambre.
  3. Appareil de séchage selon l'une quelconque des revendications précédentes,
    caractérisé en ce
    que les plaques de chauffage/de refroidissement (4) sont reliées à la paroi (6) de la chambre de manière à être étanches au vide.
  4. Appareil de séchage selon l'une quelconque des revendications
    précédentes,
    caractérisé en ce
    que les surfaces de chauffage/de refroidissement (4 ; 4') sont reliées mécaniquement à la face intérieure de la paroi (6) de la chambre par des pièces d'écartement (5) et qu'elles forment avec cette paroi une fente plane apte à être évacuée. Des raccordements sous vide sont prévus dans la paroi (6) de la chambre.
  5. Appareil de séchage selon l'une quelconque des revendications
    précédentes,
    caractérisé en ce
    que la fente est réglable sur le niveau de pression de la chambre de séchage par un système à vide afin de compenser la pression.
  6. Appareil de séchage selon l'une quelconque des revendications
    précédentes,
    caractérisé en ce
    que les pièces d'écartement (5) sont réalisées en un matériau peu conducteur de chaleur, notamment en acier inoxydable.
  7. Appareil de séchage selon l'une quelconque des revendications
    précédentes,
    caractérisé en ce
    que des tôles de liaison (9) élastiques entre des plaques de chauffage/de refroidissement (4 ; 4') et la paroi (6) de la chambre sont réalisées de manière si flexible que les variations de longueur dues à la température des surfaces de chauffage/de refroidissement sont compensées sans endommagement du matériau.
  8. Appareil de séchage selon l'une quelconque des revendications
    précédentes,
    caractérisé en ce
    que la chambre de séchage (23) est apte à être évacuée pendant le processus de congélation même afin de réduire les influences de convection.
  9. Appareil de séchage selon l'une quelconque des revendications
    précédentes,
    caractérisé en ce
    que les systèmes de type CIP/SIP sont montés de manière à pouvoir nettoyer toutes les surfaces.
  10. Appareil de séchage selon l'une quelconque des revendications
    précédentes,
    caractérisé en ce
    que les systèmes de régulation de température des plaques de chauffage/de refroidissement sont aptes à être réglés à la température appropriée, commandés par capteurs.
  11. Appareil de séchage selon l'une quelconque des revendications précédentes,
    caractérisé en ce
    que les systèmes de régulation de température des plaques de chauffage/de refroidissement sont aptes à être réglés à la température appropriée de manière prédictive, commandés par un programme de calcul.
  12. Appareil de séchage selon l'une quelconque des revendications 1 à 9,
    caractérisé en ce
    que les systèmes de régulation de température des plaques de chauffage/de refroidissement sont aptes à être réglés à la température appropriée, commandés par un système hybride constitué d'un capteur et d'un ordinateur.
  13. Procédé de séchage de matière humide en utilisant un appareil de séchage (1) selon l'une quelconque des revendications 1 à 12, avec les étapes :
    stériliser, le cas échéant à chaud, la chambre (23) y compris les plaques de positionnement (2) vides,
    charger les plaques de positionnement (2) de matière humide ou de récipients (3) contenant la matière humide,
    fermer l'ouverture de la chambre et refroidir les plaques de positionnement (2) avec refroidissement simultané des plaques de chauffage/de refroidissement (4 ; 4'),
    ensuite, évacuer et exécuter un programme de température afin de réchauffer graduellement les plaques de positionnement (2) et
    adaptation progressive simultanée de la température des plaques de chauffage/de refroidissement (4 ; 4') à la température des récipients (3) ou de la matière humide, ventiler le dispositif avec un gaz stérile, régler la température des plaques de positionnement (2) et des plaques de chauffage/de refroidissement (4 ; 4'), sur la température de déchargement, le cas échéant sur la température ambiante, le cas échéant refermer les récipients (3) et retirer les récipients (3) ou la matière humide.
EP03722477A 2002-04-23 2003-04-15 Dispositif de lyophilisation Expired - Lifetime EP1502063B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE10218007A DE10218007A1 (de) 2002-04-23 2002-04-23 Gefriertrockenvorrichtung
DE10218007 2002-04-23
PCT/EP2003/003893 WO2003091645A1 (fr) 2002-04-23 2003-04-15 Dispositif de lyophilisation

Publications (2)

Publication Number Publication Date
EP1502063A1 EP1502063A1 (fr) 2005-02-02
EP1502063B1 true EP1502063B1 (fr) 2010-02-24

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EP03722477A Expired - Lifetime EP1502063B1 (fr) 2002-04-23 2003-04-15 Dispositif de lyophilisation

Country Status (18)

Country Link
US (1) US6931754B2 (fr)
EP (1) EP1502063B1 (fr)
JP (1) JP2005524041A (fr)
KR (1) KR101026067B1 (fr)
CN (1) CN100554842C (fr)
AT (1) ATE458973T1 (fr)
AU (1) AU2003229670B2 (fr)
BR (1) BRPI0309662A2 (fr)
CA (1) CA2483152C (fr)
DE (2) DE10218007A1 (fr)
DK (1) DK1502063T3 (fr)
ES (1) ES2337777T3 (fr)
IL (2) IL164740A0 (fr)
MX (1) MXPA04010416A (fr)
NZ (1) NZ536051A (fr)
RU (1) RU2004134330A (fr)
WO (1) WO2003091645A1 (fr)
ZA (1) ZA200408489B (fr)

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US8434240B2 (en) 2011-01-31 2013-05-07 Millrock Technology, Inc. Freeze drying method
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CN103335507A (zh) * 2013-06-21 2013-10-02 上海东富龙制药设备制造有限公司 一种用于真空冷冻干燥机的灭菌冷却装置
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CN105091508B (zh) * 2015-08-26 2017-06-23 楚天科技股份有限公司 一种冻干机
US10605527B2 (en) * 2015-09-22 2020-03-31 Millrock Technology, Inc. Apparatus and method for developing freeze drying protocols using small batches of product
US10113797B2 (en) 2016-09-09 2018-10-30 Sp Industries, Inc. Energy recovery in a freeze-drying system
CN106889058B (zh) * 2017-02-20 2019-07-19 徐小杨 一种细胞冻干系统和方法
CN112005069B (zh) * 2018-04-10 2023-01-10 Ima生命北美股份有限公司 冷冻干燥处理和装备健康状况监测
US11744257B1 (en) * 2018-10-19 2023-09-05 Harvest Right, LLC Freeze-drying methods including vacuum freezing
JP7312730B2 (ja) * 2020-07-17 2023-07-21 エスペック株式会社 環境形成装置
US11287185B1 (en) 2020-09-09 2022-03-29 Stay Fresh Technology, LLC Freeze drying with constant-pressure and constant-temperature phases
CN112240682A (zh) * 2020-10-14 2021-01-19 中南大学 一种可用于连续生产的喷雾冷冻干燥装置
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Also Published As

Publication number Publication date
CA2483152C (fr) 2010-10-19
IL164740A (en) 2012-08-30
KR101026067B1 (ko) 2011-04-04
IL164740A0 (en) 2005-12-18
CN100554842C (zh) 2009-10-28
JP2005524041A (ja) 2005-08-11
DE10218007A1 (de) 2003-11-06
DK1502063T3 (da) 2010-05-31
DE50312444D1 (de) 2010-04-08
EP1502063A1 (fr) 2005-02-02
ZA200408489B (en) 2005-12-28
AU2003229670A1 (en) 2003-11-10
WO2003091645A1 (fr) 2003-11-06
MXPA04010416A (es) 2005-03-07
US20040060191A1 (en) 2004-04-01
ES2337777T3 (es) 2010-04-29
US6931754B2 (en) 2005-08-23
CN1682083A (zh) 2005-10-12
BRPI0309662A2 (pt) 2016-07-05
KR20040106366A (ko) 2004-12-17
NZ536051A (en) 2006-07-28
ATE458973T1 (de) 2010-03-15
CA2483152A1 (fr) 2003-11-06
AU2003229670B2 (en) 2009-01-08
RU2004134330A (ru) 2005-07-20

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