EP0546931A1 - Gefriertrocknungsanlage - Google Patents

Gefriertrocknungsanlage Download PDF

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Publication number
EP0546931A1
EP0546931A1 EP92403331A EP92403331A EP0546931A1 EP 0546931 A1 EP0546931 A1 EP 0546931A1 EP 92403331 A EP92403331 A EP 92403331A EP 92403331 A EP92403331 A EP 92403331A EP 0546931 A1 EP0546931 A1 EP 0546931A1
Authority
EP
European Patent Office
Prior art keywords
circuit
installation
lyophilization
shelves
trap
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.)
Granted
Application number
EP92403331A
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English (en)
French (fr)
Other versions
EP0546931B1 (de
Inventor
Guy Beurel
Serge Beurel
Gilles Beurel
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Individual
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Individual
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 Individual filed Critical Individual
Publication of EP0546931A1 publication Critical patent/EP0546931A1/de
Application granted granted Critical
Publication of EP0546931B1 publication Critical patent/EP0546931B1/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 lyophilization installation.
  • Lyophilization devices are installations intended to dry products, generally organic, by sublimation at very low temperature and very low pressure.
  • Freeze-dryers are devices comprising two enclosures: a first, in which the products to be treated are arranged and next to it, a second in which is arranged an organ called a trap, intended to receive the water coming from the products.
  • the installation also includes a set of vacuum and cold generating devices and circulation pumps for heat transfer fluids which carry the shelves and the trap at determined temperatures causing sublimation.
  • the temperatures in the chambers are regulated separately by two independent heat and / or cold production circuits.
  • the enclosure, where the products are stored, or desiccation enclosure is crossed by a first circuit supplied with a refrigerating liquid such as that marketed under the name "Freon” and regulated in temperature by a production center for cold and hot of so as to ensure the cooling of the shelves and the freezing of the product, then to heat them to bring the product to the temperatures of primary lyophilization (approximately - 20 ° C) and secondary (approximately 30 ° C).
  • the enclosure where the trap is located is crossed by a second circuit supplied with a silicone liquid and regulated in temperature by a plurality of power stations arranged in parallel, each comprising in known manner a condenser and a Freon exchanger.
  • the choice of different refrigerants is mainly due to the fact that the performances requested from the circuits are different: the first circuit must both go down to a very low temperature (about -45 to -50 ° C for freezing) but for a short time, and high (+ 30 ° C) while the second must ensure only a very low temperature (about -50 to -70 ° C ) for several hours.
  • the advantage of such a device is that it is possible to choose refrigeration devices that precisely meet the specific working conditions and offer an optimal performance ratio.
  • the major drawback is that the first circuit is direct expansion and it is difficult to properly control the heat exchange in the first enclosure, that is to say, lyophilization.
  • a desiccation device comprising a single refrigerant, more precisely a fluid called R11; this device describes a patent US-A-3 656 240, includes a cold generator which supplies the two speakers in parallel.
  • Each portion of the circuit includes a circulation pump which allows the flow rate in each enclosure to be controlled, but this installation does not allow precise control of the heat exchanges.
  • the liquid used cannot be brought to a high temperature above 60 ° C. while maintaining low pressures, of the order of atmospheric pressure. It is therefore impossible to sterilize the speakers with R11 fluid.
  • the desiccation chambers used for very delicate products such as pharmaceuticals must imperatively be free from any equivalent bacteria or pathogenic particle, which is obtained by hot sterilization.
  • the US device cannot therefore be used.
  • the object of the invention is to resolve the above drawbacks in order to produce a very precise device for regulating heat production by using a device of the type described in US Pat. No. 3,656,240, that is to say using a the same fluid in any installation.
  • the installation comprises two or two-n lyophilization groups, the drying chambers being contiguous in pairs and connected by a communication line controlled by a valve.
  • This variant makes it possible to operate alternately on one or the other freeze-drying group and thus allows almost continuous production.
  • the lyophilization installation mainly comprises two enclosures, the desiccation enclosure 1 comprising the shelves 5 on which the products to be dried are placed, and the enclosure 2 where the trap 6 is located on which the the water contained in the products must migrate; enclosures 1 and 2 communicate via a pipe 3 controlled by a valve 4.
  • the installation comprises a main temperature regulation circuit 7 forming a closed circuit 7.
  • This circuit includes a cold production unit 16 and a circulation pump 14 so that the temperature regulation in cold is continuous and independent. any secondary circuit (freeze-drying groups).
  • This main circuit 7 is intended to supply one or more lyophilization groups mounted in parallel.
  • this problem is solved by using, for the main circuit, large section pipes, diameter of the order of at least 100 millimeters, the pipe itself then constituting the heat reservoir.
  • the main circuit supplies a lyophilization group.
  • Each group comprises in parallel on the main circuit 7 a primary bypass 9 which passes through the trap, and a secondary bypass 8 which passes through the shelves.
  • the secondary bypass 8 is connected to the main circuit by the inlet 20 and outlet 21 pipes, each provided with isolation valves 10 and 12.
  • valves 81 and 82 comprising a circulation pump 13, a thermal regulation assembly (hot and cold) 15.
  • the lines 8 and 80 form a secondary circuit, independent of the main circuit 7.
  • the central control unit 15 includes a refrigeration unit 83 and a heater 84.
  • the main circuit 7 comprises in parallel a series of refrigeration production plants 16. This arrangement makes it possible both to remedy untimely damage to a power station, during treatment and to have greater flexibility of power, and consequently this arrangement makes it possible to supply several lyophilization groups as shown in FIG. 4.
  • the installation comprises two conduits 85,86 controlled by valves 87,88 which connect the bypass supplying the trap to the secondary circuit.
  • This extension is intended to use the thermal group 15 for reheating the trap and its discharge of water and for cooling the trap after sterilization.
  • the installation comprises two lyophilization groups mounted in parallel on the main pipe 7 and supplied by the refrigeration unit 16 and the pump 14.
  • the drying chambers 1 and 1 ′ are mounted contiguous and there is provided between them a communication line 89 controlled by a set of valves 100.
  • the secondary circuits are also interconnected so as to ensure identical thermal regulation in all the pipes.
  • the device operates as follows (in FIG. 3 the parts in strong lines are the active circuit elements):
  • the dry products are cooled with the cold plant 83.
  • the fluid of the secondary loop is used for cooling: the trap of the main circuit is isolated and it is fed by extension 87.88 of the secondary circuit.
  • the fluid in the secondary circuit 8, 80 is then cooled by the cooling unit 83.

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)
EP19920403331 1991-12-12 1992-12-09 Gefriertrocknungsanlage Expired - Lifetime EP0546931B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR9115463 1991-12-12
FR9115463A FR2685066B1 (fr) 1991-12-12 1991-12-12 Dispositif de lyophilisation.

Publications (2)

Publication Number Publication Date
EP0546931A1 true EP0546931A1 (de) 1993-06-16
EP0546931B1 EP0546931B1 (de) 1995-09-27

Family

ID=9419993

Family Applications (1)

Application Number Title Priority Date Filing Date
EP19920403331 Expired - Lifetime EP0546931B1 (de) 1991-12-12 1992-12-09 Gefriertrocknungsanlage

Country Status (5)

Country Link
EP (1) EP0546931B1 (de)
JP (1) JPH06174367A (de)
CA (1) CA2085069A1 (de)
DE (1) DE69205127T2 (de)
FR (1) FR2685066B1 (de)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0989376A3 (de) * 1998-09-21 2000-04-12 Praxair Technology, Inc. Gefriertrocknung mit reduziertem Kryogenmittelverbrauch
WO2001014809A1 (en) * 1999-08-23 2001-03-01 3M Innovative Properties Company Apparatus using halogenated organic heat transfer fluids
WO2008085208A2 (en) * 2006-09-08 2008-07-17 Praxair Technology, Inc. Cryogenic refrigeration system for lyophilization
EP3015804A4 (de) * 2013-06-27 2016-09-21 Maekawa Seisakusho Kk Gefriertrocknungssystem und gefriertrocknungsverfahren

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104132529B (zh) * 2014-07-25 2016-05-25 上海共和真空技术有限公司 用于三重热交换板式冻干机的导热油冷却方法

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2025999A1 (de) * 1969-05-30 1970-12-03 N.V. Philips' Gloeilampenfabrieken, Eindhoven (Niederlande) Gefriertrocknungsanlage
FR2461213A1 (fr) * 1979-07-04 1981-01-30 Kyowa Vacuum Eng Appareil a vide, notamment pour la conservation des produits alimentaires

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2025999A1 (de) * 1969-05-30 1970-12-03 N.V. Philips' Gloeilampenfabrieken, Eindhoven (Niederlande) Gefriertrocknungsanlage
FR2461213A1 (fr) * 1979-07-04 1981-01-30 Kyowa Vacuum Eng Appareil a vide, notamment pour la conservation des produits alimentaires

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
ADAMS G. D. J.: "FREEZE-DRYING OF BIOLOGICAL MATERIALS.", DRYING TECHNOLOGY., TAYLOR & FRANCIS, PHILADELPHIA, PA., US, vol. 09., no. 04., 1 September 1991 (1991-09-01), US, pages 891 - 925., XP000232604, ISSN: 0737-3937 *

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0989376A3 (de) * 1998-09-21 2000-04-12 Praxair Technology, Inc. Gefriertrocknung mit reduziertem Kryogenmittelverbrauch
WO2001014809A1 (en) * 1999-08-23 2001-03-01 3M Innovative Properties Company Apparatus using halogenated organic heat transfer fluids
US6610250B1 (en) 1999-08-23 2003-08-26 3M Innovative Properties Company Apparatus using halogenated organic fluids for heat transfer in low temperature processes requiring sterilization and methods therefor
WO2008085208A2 (en) * 2006-09-08 2008-07-17 Praxair Technology, Inc. Cryogenic refrigeration system for lyophilization
WO2008085208A3 (en) * 2006-09-08 2009-02-12 Praxair Technology Inc Cryogenic refrigeration system for lyophilization
US8015841B2 (en) 2006-09-08 2011-09-13 Praxair Technology, Inc. Cryogenic refrigeration system for lyophilization
US8938979B2 (en) 2006-09-08 2015-01-27 Praxair Technology, Inc. Method for lyophilization using cryogenic refrigeration system
EP3015804A4 (de) * 2013-06-27 2016-09-21 Maekawa Seisakusho Kk Gefriertrocknungssystem und gefriertrocknungsverfahren
US10309723B2 (en) 2013-06-27 2019-06-04 Mayekawa Mfg.Co., Ltd. Freeze-drying system and freeze-drying method

Also Published As

Publication number Publication date
JPH06174367A (ja) 1994-06-24
EP0546931B1 (de) 1995-09-27
DE69205127D1 (de) 1995-11-02
DE69205127T2 (de) 1996-05-30
FR2685066B1 (fr) 1995-04-14
CA2085069A1 (fr) 1993-06-13
FR2685066A1 (fr) 1993-06-18

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