EP0317411B1 - Vorrichtung zur Gefriertrocknung mit Mitteln zur Bildung einer aktiven thermischen Abschirmung zwischen den Gefriertrocknungsregalen - Google Patents

Vorrichtung zur Gefriertrocknung mit Mitteln zur Bildung einer aktiven thermischen Abschirmung zwischen den Gefriertrocknungsregalen Download PDF

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Publication number
EP0317411B1
EP0317411B1 EP88402845A EP88402845A EP0317411B1 EP 0317411 B1 EP0317411 B1 EP 0317411B1 EP 88402845 A EP88402845 A EP 88402845A EP 88402845 A EP88402845 A EP 88402845A EP 0317411 B1 EP0317411 B1 EP 0317411B1
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EP
European Patent Office
Prior art keywords
freeze
drying
shelves
heating
plates
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
EP88402845A
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English (en)
French (fr)
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EP0317411A1 (de
Inventor
René Gimeno
Alain Huc
Pierre Devictor
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.)
BASF Beauty Care Solutions France SAS
Original Assignee
Coletica SA
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Filing date
Publication date
Application filed by Coletica SA filed Critical Coletica SA
Priority to AT88402845T priority Critical patent/ATE79461T1/de
Publication of EP0317411A1 publication Critical patent/EP0317411A1/de
Application granted granted Critical
Publication of EP0317411B1 publication Critical patent/EP0317411B1/de
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    • 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 present invention relates to a lyophilization device comprising means forming an active heat shield between the lyophilization shelves.
  • Lyophilization is a drying technique involving freezing and then sublimation of the water contained in the frozen product.
  • Lyophilization can be achieved by two types of apparatus: the first consists of balloons located in the atmosphere and connected to the vacuum enclosure containing the trap. In this system, the substance is previously frozen in the flask placed to do this in a freezer. In this system, the calories necessary for sublimation are provided by the atmosphere.
  • the second type of device consists of shelves on which the product to be lyophilized is placed. The product can be pre-frozen or frozen in situ on the shelves. When the freezing is finished, the lyophilization is carried out on the same shelves which will be heated so as to provide the product with the calories necessary for the sublimation of the water.
  • the first phenomenon comes from the imprisonment of a certain quantity of liquid between an envelope of ice forming on the bottom, the walls of the tray containing the substance as well as on the surface of the product.
  • the frigories on the bottom and the walls are brought by conduction from the shelf of the freeze dryer while on the surface of the product, they are brought mainly by radiation from the upper shelf.
  • an increase in volume occurs and the liquid passes through the frozen wall of the surface and forms a mound which freezes ( Figure 1).
  • the second phenomenon that is to say the formation of a crust on the surface of the product is caused by thawing due to radiant heating of the freeze dryer shelf located just above the freeze drying tray, and the absence of sufficient thermal conduction inside the product.
  • This thawing results in the liquefaction of the water in the product which no longer sublimates but then evaporates. This results in the formation of a more compact crust on the surface of the product which makes the lyophilized material heterogeneous.
  • this crust is relatively waterproof. It can in certain cases contribute to lengthening the freeze-drying time by slowing down the exchanges between the gas and the deeper layers of frozen product.
  • US Patent 4,501,719 relates to a lyophilization device comprising a particular plate 14 provided with housings 12 in which the solutions 16 to be lyophilized are arranged.
  • a lyophilization device comprising a particular plate 14 provided with housings 12 in which the solutions 16 to be lyophilized are arranged.
  • lines 62 to 68 and in column 4, lines 50 to 58 it is mentioned the use of an insulating plate 43 placed above the plate 14 containing the lyophilized solutions disposed in the housings or wells 12 (see Figure 3).
  • This insulating plate 43 is made of Styrofoam with an intermediate plexiglass sheet 44. It is preferably wrapped in a aluminum foil to increase its insulation properties (column 4, lines 50 to 53).
  • the present invention therefore aims to solve the new technical problem consisting in the supply of a solution making it possible to obtain, by lyophilization, lyophilized products which are homogeneous, or with greatly improved homogeneity, compared to the products obtained by the lyophilization processes and apparatus. previously known.
  • the main object of the present invention is also to solve the new technical problem consisting in providing a solution making it possible to obtain, by lyophilization, various viscous products or solutions, very difficult to lyophilize, making it possible to obtain very homogeneous and plans.
  • the main object of the present invention is also to solve the new technical problem consisting in the supply of a solution making it possible to obtain by freeze-drying products or various solutions, in particular viscous solutions, even when placed in great thickness, leading to products homogeneous freeze-dried.
  • the present invention also aims to solve the new technical problem consisting in the supply of a solution making it possible to obtain, by freeze-drying, products or various solutions, in particular viscous solutions, which can be arranged in great thickness, leading to products homogeneous, extremely simple design, low manufacturing cost, usable on an industrial scale.
  • the present invention provides an apparatus for lyophilization of various products or solutions, in particular viscous solutions, which can be arranged in great thickness, comprising lyophilization shelves placed inside a lyophilization enclosure, on which one can put products or solutions to be lyophilized, which may be contained in open containers, as well as associated cooling and / or heating means, preferably made incorporated, into said shelves, characterized in that means forming an active thermal screen are disposed between said lyophilization shelves, comprising heating and / or cooling means, thus making it possible to slow down the heat exchanges between the surface of the product to be lyophilized and the heating and / or cooling elements associated with the shelves.
  • these means forming an active screen can be produced in the form of plates, advantageously of a shape adapted to the lyophilization shelves, and can be fixed under said shelves, that is to say opposite to the products. freeze-drying resting on said shelf.
  • these plates constituting the means forming an active screen contain heating resistors.
  • these plates contain, embedded in the mass, elements capable of heating during freezing and of cooling during the lyophilization proper (step of sublimation of water).
  • the plates constituting the active screen means are hollow and are provided to allow the circulation of a heat transfer fluid inside said plates.
  • the apparatus is characterized in that the calories or the heat transfer fluid circulating inside the plates forming the screen originate from the heating and cooling system freeze-drying trays, the calories used being those supplied by the refrigeration unit during the cooling of the freezing operation while during the freeze-drying period, on the contrary, the frigories are sent to the active screen plates and the calories in the freeze-drying trays.
  • the lyophilization device according to the invention, it is characterized in that the calories of the heat transfer fluid circulating inside the plates forming an active screen come from an autonomous, internal heating system or external to the freeze dryer.
  • the lyophilization device represented by the general reference number 1 conventionally comprises shelves 2, on which are placed various products or solutions to be lyophilized 4, possibly contained in open containers 6.
  • These shelves 2 are usually equipped with heating and cooling means, making it possible to carry out the freezing step, then the step of sublimation of the water contained in the frozen product.
  • the shelves 2 are made hollow and a heat transfer product is circulated inside them brought either to the temperature necessary for freezing the products, or to the temperature necessary for the sublimation of the water.
  • a crust forms on the surface of the product caused by thawing due to radiation heating of the freeze dryer shelf located just above the freeze drying tray on which the product rests, and the absence of sufficient thermal conduction inside the product.
  • a more compact crust is formed on the surface of the product, which makes the lyophilized product heterogeneous.
  • FIG 2 there is shown a lyophilization apparatus according to the invention referenced 10, which also includes lyophilization shelves 12, which may be identical to those of the lyophilization apparatus shown in Figure 1, as described below -above.
  • this lyophilization device 10 comprises means forming an active thermal screen 14, arranged between the shelves 12, as is clearly understandable from FIG. 2.
  • these means forming an active screen can take the form of plates.
  • the plates constituting the means forming an active screen comprise heating means and / or cooling means.
  • These heating means can be formed by simple heating resistors.
  • the heating and / or cooling means of the screen forming means 14 can be constituted by a heat transfer fluid circulating in the plates which are then made hollow.
  • This device operates according to the method previously described; thus, heating is carried out inside the screen means during freezing. This advantageously slows down the heat exchange between the surface of the product and the cooling elements of the lyophilization device, contained in the shelves, during the freezing step.
  • the means forming an active screen cool down during the lyophilization stage proper, which is controlled so that the temperature of the frozen product rises gradually.
  • the heating means of the active screen means 14, constituted by heating resistors, with a power of 225W / m2 are supplied with a voltage of 220V.
  • the power supply is stopped and freeze-drying is started.
  • a vacuum of 0.3 mb is created in the enclosure of the freeze dryer and the shelves are heated so that the temperature of the frozen product is maintained at -25 ° C.
  • This last phase lasts approximately 16 hours.
  • secondary desiccation during which the vacuum is lowered to 10 ⁇ 2mb and the product temperature raised to 40 ° C. This operation takes approximately 3 hours.
  • two layers of 2mm thick are split: one from the side of the biomaterial which was turned towards the upper shelf during the lyophilization, and the other from the side in contact with the tray placed on the cooling and heating shelf. These two layers were weighed for five different lyophilizations.
  • the first results are also to be compared with those obtained by the same freeze dryer equipped with passive screen means made only of an insulating material.
  • the invention is particularly advantageous on the one hand, in the case of lyophilization of viscous solutions inside which the heat exchanges by convection are very difficult, and on the other hand, in the case of lyophilization of large thicknesses which prevent rapid heat exchanges between the face of the product in contact with the freeze dryer shelf and the surface.
  • the material constituting the plates is a thermally conductive material, advantageously a metal, for example anodized aluminum or a steel. stainless.
  • the lyophilization device it is characterized in that the calories or the heat transfer fluid circulating inside the plates forming an active screen come from the system for heating and cooling the plates freeze-drying, the calories used being those supplied by a refrigeration unit during the cooling of the freezing operation, while during the freeze-drying period, on the contrary, the frigories are sent to the plates forming an active screen and the calories to the trays lyophilization.
  • the lyophilization device according to the invention, it is characterized in that the calories of the heat-transfer fluid circulating inside the plates forming an active screen come from an autonomous heating system, internal or external to the freeze dryer.

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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)
  • Freezing, Cooling And Drying Of Foods (AREA)

Claims (7)

1. Apparat zur Lyophilisierung verschiedener Produkte oder Lösungen, insbesondere viskoser Lösungen, die in großer Dicke aufgebracht werden können, umfassend innerhalb eines Lyophilisationsgehäuses angeordnete Lyophilisationsetagere, auf die zu lyophilisierende Produkte oder Lösungen gegeben werden können, welche in offenen Behältern enthalten sein können, sowie mit den Etageren kombinierte, vorzugsweise in diesen inkorporierte Einrichtungen zum Kühlen und/oder Erhitzen, dadurch gekennzeichnet, daß einen aktiven Wärmeschild bildende Einrichtungen zwischen den Lyophilisationsetageren angeordnet sind und Heiz- und/oder Kühlmittel umfassen, wodurch es möglich ist, den Wärmeaustausch zwischen der Oberfläche des zu lyophilisierenden Produkts und den mit den Etageren kombinierten Heiz- und/oder Kühleinrichtungen zu verzögern.
2. Lyophilisationsapparat nach Anspruch 1, dadurch gekennzeichnet, daß die Heizmittel der einen aktiven Schild bildenden Einrichtungen während der Einfrierphase und die Kühlmittel der einen aktiven Schild bildenden Einrichtungen während der eigentlichen Lyophilisationsphase in Betrieb gesetzt sind.
3. Lyophilisationsapparat nach Anspruch 1 oder 2, dadurch gekennzeichnet, daß die einen Schild bildenden Einrichtungen in Form von vorteilhafterweise formmäßig an die Lyophilisationsetagere angepaßten Platten ausgebildet und unter den Etageren befestigt sein können.
4. Lyophilisationsapparat nach den Ansprüchen 1 bis 3, dadurch gekennzeichnet, daß die Platten, die die einen aktiven Schild bildenden Einrichtungen darstellen, Heizwiderstände einschließen.
5. Lyophilisationsapparat nach den Ansprüchen 1 bis 4, dadurch gekennzeichnet, daß die Platten, die die einen aktiven Schild bildenden Einrichtungen darstellen, hohl sind und zur Gewährleistung des Umlaufs eines flüssigen Kühlmittels innerhalb der Platten vorgesehen sind.
6. Lyophilisationsapparat nach einem der Ansprüche 1 bis 5, dadurch gekennzeichnet, daß die Wärme oder das Kühlmittel, die bzw. das innerhalb der einen aktiven Schild bildenden Platten zirkuliert, vom Heiz- bzw. Kühlsystem der Lyophilisationsplatten kommen, wobei die verwendete Wärme jene ist, die von einer Gefriergruppe während der Kühlung beim Gefrierschritt kommt, wobei hingegen während der Lyophilisationsperiode die Kälte in die einen aktiven Schild bildenden Platten und die Wärme in die Lyophilisationsplatten geleitet wird.
7. Lyophilisationsapparat nach einem der Ansprüche 1 bis 5, dadurch gekennzeichnet, daß die Wärme des innerhalb der einen aktiven Schild bildenden Platten zirkulierenden Kühlmittels von einem autonomen Heizsystem innerhalb oder außerhalb des Lyophilisators kommt.
EP88402845A 1987-11-17 1988-11-14 Vorrichtung zur Gefriertrocknung mit Mitteln zur Bildung einer aktiven thermischen Abschirmung zwischen den Gefriertrocknungsregalen Expired - Lifetime EP0317411B1 (de)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT88402845T ATE79461T1 (de) 1987-11-17 1988-11-14 Vorrichtung zur gefriertrocknung mit mitteln zur bildung einer aktiven thermischen abschirmung zwischen den gefriertrocknungsregalen.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR8715880A FR2623277B1 (fr) 1987-11-17 1987-11-17 Procede et appareil de lyophilisation comportant des moyens formant ecran thermique entre les etageres de lyophilisation
FR8715880 1987-11-17

Publications (2)

Publication Number Publication Date
EP0317411A1 EP0317411A1 (de) 1989-05-24
EP0317411B1 true EP0317411B1 (de) 1992-08-12

Family

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Application Number Title Priority Date Filing Date
EP88402845A Expired - Lifetime EP0317411B1 (de) 1987-11-17 1988-11-14 Vorrichtung zur Gefriertrocknung mit Mitteln zur Bildung einer aktiven thermischen Abschirmung zwischen den Gefriertrocknungsregalen

Country Status (9)

Country Link
US (1) US4953299A (de)
EP (1) EP0317411B1 (de)
JP (1) JP2545592B2 (de)
AT (1) ATE79461T1 (de)
CA (1) CA1320428C (de)
DE (2) DE317411T1 (de)
ES (1) ES2010175T3 (de)
FR (1) FR2623277B1 (de)
GR (1) GR3005923T3 (de)

Families Citing this family (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5519946A (en) * 1992-03-12 1996-05-28 The Boc Group, Inc. Freeze dryer shelf
DE4421421C2 (de) * 1993-12-24 1996-08-29 Daimler Benz Aerospace Airbus Trocknungsverfahren für Bauteile aus faserverstärkten Kunststoffen
DE19751031A1 (de) 1997-11-19 1999-06-24 Ingo Dipl Ing Heschel Verfahren zur Herstellung poröser Strukturen
US6454787B1 (en) 1998-12-11 2002-09-24 C. R. Bard, Inc. Collagen hemostatic foam
US6361551B1 (en) 1998-12-11 2002-03-26 C. R. Bard, Inc. Collagen hemostatic fibers
US6434913B1 (en) 2000-09-15 2002-08-20 Thomas Hatch Single-use syringe
US7347004B1 (en) 2005-01-13 2008-03-25 Lyophilization Services Of New England, Inc. Freeze drying apparatus and method
GB0525115D0 (en) * 2005-12-09 2006-01-18 Oxford Biosensors Ltd Freeze drying of target substances
WO2009006891A1 (en) * 2007-07-10 2009-01-15 Niro A/S Method for freeze-drying a product and freeze-drying apparatus for carrying out the method
DE102009008970A1 (de) * 2008-12-04 2010-06-10 Walter Wiedenmannott Gefriertrockner und Verfahren zum Betrieb eines Gefriertrockners
US8371039B2 (en) * 2009-12-30 2013-02-12 Baxter International Inc. Thermal shielding to optimize lyophilization process for pre-filled syringes or vials
GB2482166A (en) * 2010-07-22 2012-01-25 Tissue Science Lablratories Ltd Manufacture of collagenous material from use in therapy from collagen particles
ES2621017T3 (es) 2010-09-28 2017-06-30 Baxter International Inc Optimización de la nucleación y cristalización en la liofilización utilizando una congelación con intersticios
US8966782B2 (en) 2010-09-28 2015-03-03 Baxter International Inc. Optimization of nucleation and crystallization for lyophilization using gap freezing
GB2516191A (en) * 2012-03-28 2015-01-14 Baxter Int Optimization of nucleation and crystallization for lyophilization using gap freezing

Family Cites Families (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2602825A (en) * 1948-01-24 1952-07-08 Stokes Machine Co Sublimation process and apparatus
US3118742A (en) * 1958-08-22 1964-01-21 Nat Res Dev Vacuum food press drier
US3135589A (en) * 1961-09-29 1964-06-02 Pennsalt Chemicals Corp Drying apparatus
FR2284842A1 (fr) * 1974-09-11 1976-04-09 Nestle Sa Perfectionnement apporte la lyophilisation des produits solides, liquides ou pateux
JPS6015867B2 (ja) * 1980-07-04 1985-04-22 日本真空技術株式会社 真空凍結乾燥装置
US4501719A (en) * 1981-05-04 1985-02-26 Marquest Medical Products, Inc. Tray apparatus for freeze-drying biologicals having a predetermined unit dosage
JPS5935242B2 (ja) * 1981-10-29 1984-08-28 山之内製薬株式会社 凍結乾燥機の棚

Also Published As

Publication number Publication date
DE3873695T2 (de) 1993-01-21
CA1320428C (en) 1993-07-20
US4953299A (en) 1990-09-04
FR2623277A1 (fr) 1989-05-19
DE3873695D1 (de) 1992-09-17
ES2010175A4 (es) 1989-11-01
JPH02110281A (ja) 1990-04-23
ES2010175T3 (es) 1993-04-01
EP0317411A1 (de) 1989-05-24
JP2545592B2 (ja) 1996-10-23
FR2623277B1 (fr) 1990-04-27
GR3005923T3 (de) 1993-06-07
DE317411T1 (de) 1989-11-16
ATE79461T1 (de) 1992-08-15

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