EP0301117B1 - Einrichtung zur Gefriertrocknung - Google Patents

Einrichtung zur Gefriertrocknung Download PDF

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Publication number
EP0301117B1
EP0301117B1 EP87110955A EP87110955A EP0301117B1 EP 0301117 B1 EP0301117 B1 EP 0301117B1 EP 87110955 A EP87110955 A EP 87110955A EP 87110955 A EP87110955 A EP 87110955A EP 0301117 B1 EP0301117 B1 EP 0301117B1
Authority
EP
European Patent Office
Prior art keywords
valve
chamber
condensation surface
condensor
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.)
Expired - Lifetime
Application number
EP87110955A
Other languages
German (de)
English (en)
French (fr)
Other versions
EP0301117A1 (de
Inventor
Heinrich Steinkamp
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
Amsco Finn Aqua 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
Family has litigation
First worldwide family litigation filed litigation Critical https://patents.darts-ip.com/?family=8197162&utm_source=google_patent&utm_medium=platform_link&utm_campaign=public_patent_search&patent=EP0301117(B1) "Global patent litigation dataset” by Darts-ip is licensed under a Creative Commons Attribution 4.0 International License.
Application filed by Finn Aqua Santasalo Sohlberg GmbH, Amsco Finn Aqua GmbH filed Critical Finn Aqua Santasalo Sohlberg GmbH
Priority to ES87110955T priority Critical patent/ES2068809T3/es
Priority to EP87110955A priority patent/EP0301117B1/de
Priority to DE3750847T priority patent/DE3750847D1/de
Priority to JP63173852A priority patent/JP2676374B2/ja
Priority to US07/226,536 priority patent/US4949473A/en
Publication of EP0301117A1 publication Critical patent/EP0301117A1/de
Application granted granted Critical
Publication of EP0301117B1 publication Critical patent/EP0301117B1/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 present invention relates to a device for freeze drying with an evacuable chamber and an evacuation system.
  • 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 takes place approximately as follows: after freezing the product containing water, the sublimation of the water present in ice form takes place under vacuum (about 10 perennial1 mbar). After this main drying, the post-drying takes place, during which the adsorptively bound moisture is removed in order to achieve extremely low residual moisture. During the final drying, the product is warmed up in compliance with permissible temperature limits. The pressure at which post-drying takes place is around 10 ⁇ 3 mbar.
  • the prior art also includes the content of US-A-40 60 400.
  • This document discloses a truck with a cooling container and a refrigerator. Food is transported in the truck's cooling container at normal pressure. In the event of special temperature conditions or if the chiller fails liquid nitrogen is sprayed into the cooling container.
  • the present invention has for its object to provide a freeze-drying device of the type mentioned, in which the product batches are no longer at risk from accidents of the type described or a similar type.
  • the valve between the further condensation surface in the condenser and the storage container is opened, so that the refrigerant flows into the condensation surface.
  • the further condensation surface thus takes over the pumping effect.
  • the vacuum in the freeze-drying chamber remains independent of the equipment so that there is no risk of thawing or thawing of the product.
  • the additional condensation surface can be accommodated in the freeze-drying chamber, in the condenser which is usually connected to the freeze-drying chamber or in a separate chamber.
  • the device for freeze drying shown in the figure comprises the vacuum chamber 1 with the shelves 2 on which the product is located during the course of the freeze drying process.
  • the shelves 2 are usually both coolable and heatable.
  • the shelves 2 are equipped with cavities, not shown in detail, through which a temperature control agent (for example silicone oil) flows.
  • the temperature control circuit is shown in dash-dotted lines and labeled 3.
  • the setting plates 2 are parallel to each other and the feed pump 4 is switched on. If the circulating refrigerant is to be cooled, then the compressor refrigeration machine 5 is started up.
  • the compressor refrigeration machine 5 is located in the refrigerant circuit 6, which usually comprises the water-cooled condenser 7, the heat exchanger 8 and the valve 9.
  • the condenser 7 is preferably water-cooled.
  • the heat exchanger 8 is in the Temperature control circuit 3 switched on. Often, several compressor chillers are used at this point to either ensure operation (separate circuits) or to reach lower temperatures (cascade connection). It is also possible to use another chiller (for example an adsorption chiller).
  • the heating of the setting plates 2 is usually carried out by means of an electrical heating, not shown in detail, of the temperature control medium circulating in the temperature control circuit 3.
  • an electrical heating not shown in detail
  • the use of waste heat from the chillers or the use of steam-heated heat exchangers is also possible.
  • An evacuation system 11 is connected to the vacuum chamber 1 and comprises a condenser 12 and a vacuum pump 13 (gas ballast pump).
  • the valve 15 is located in the connecting line 14 between the vacuum chamber 1 and the condenser 12.
  • the line 16 with the valve 17 extends between the condenser 12 and the vacuum pump 13.
  • condensation surfaces 18 are accommodated within the condenser 12 and serve to remove water vapor from the chamber 1 during normal operation of the freeze-drying system.
  • the condensation surfaces usually consist of coils through which the refrigerant (for example chlorofluorocarbons) flows. The outer surfaces of these coils form the actual condensation surfaces.
  • the compressor refrigeration machine 5 also serves to supply the condensation surfaces 18 with refrigerant.
  • the condensation surfaces 18 can be connected to the refrigerant circuit 6 via the lines 19 and 21 with the valve 22.
  • the storage container 26 contains a low-boiling refrigerant 27, for example liquid nitrogen.
  • the line 28 is connected to the lower region of the storage container 26, which opens into its upper region above the refrigerant level.
  • an evaporator 29 and a pressure control valve 31 are switched on. With the aid of these elements, a certain pressure, for example a few bar, preferably 3 bar, can be maintained within the storage container 26.
  • An alternative in which the further condensation surface is located inside the chamber 1 is shown in dashed lines. The connected via the valve 25 to the reservoir 26 line 24 'opens into the condensation surface 23', which is arranged next to the adjusting plates 2.
  • the freeze-drying device shown works as follows: After a sterilization process, the product is introduced into the chamber 1 and frozen. For this purpose, the temperature control medium flowing in the temperature control circuit 3 is brought to correspondingly low temperatures with the aid of the compressor refrigerator 5. The valve 15 is closed during the freezing phase.
  • valves 15 and 17 are opened and the temperature control medium flowing in the temperature control circuit 3 is warmed up.
  • the valve 9 in the refrigerant circuit 6 is closed and the heating, not shown, is put into operation.
  • the chamber 1 is evacuated to a pressure of about 10 ⁇ 1 mbar.
  • the condensation surfaces 18 serve to remove the relatively large amounts of water vapor during normal operation, which are cooled with the aid of the compressor refrigerator 5. Small amounts of permanent gases still present flow through the condenser 12 and are removed using the gas ballast pump 13.
  • the cooling for the condensation surfaces 18 fails.
  • the pumping speed for water vapor decreases and returns to 0 relatively quickly.
  • the water vapor escaping from the product is no longer removed. Since the temperature control medium in the temperature control circuit 3 is warm during the main and post-drying (room temperature or slightly above), the product on the setting plates 2 begins to heat up immediately. If the product thaws or thaws, there is often a loss of quality or even a change that renders the product unusable.
  • the condensation surface 23 is provided in the condenser 12.
  • the low-boiling refrigerant 27 enters the tube coil forming the condensation surface 23 from below, evaporates there and thus cools the condensation surface 23 very quickly to relatively low temperatures.
  • the evaporated refrigerant is discharged into the atmosphere via line 32, for example.
  • the condensation surface 23 takes effect before the water vapor absorbency of the condensation surfaces 18 has significantly decreased.
  • the water vapor suction capacity of the condenser 12 is thus retained regardless of the operating medium, and that is until the refrigerant is finally used up in the storage container 26.
  • the emergency cooling can therefore be maintained for a sufficiently long time in order to be able to remedy the incident that has occurred.
  • valve 15 When an accident occurs, the valve 15 must keep its open position, close the valve 17 and open the valve 25.
  • these valves are therefore equipped with electrical or electropneumatic actuators which are designed such that the valves 15 and 25 assume their open position in the event of a power failure and the valve 17 in its closed position in the event of a power failure. This ensures a safe function of the emergency cooling device.
  • valve 25 also opens in the event of a fault, while valve 15 closes.
  • the refrigerant 27 flows via line 24 'into the condensation surface 23', evaporates there and is discharged via line 32 'into the atmosphere.
  • the condensation surface 23 ' is sufficiently cold to maintain the vacuum in the chamber 1. The product batch contained therein is therefore not endangered.

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)
EP87110955A 1987-07-29 1987-07-29 Einrichtung zur Gefriertrocknung Expired - Lifetime EP0301117B1 (de)

Priority Applications (5)

Application Number Priority Date Filing Date Title
ES87110955T ES2068809T3 (es) 1987-07-29 1987-07-29 Dispositivo para la liofilizacion.
EP87110955A EP0301117B1 (de) 1987-07-29 1987-07-29 Einrichtung zur Gefriertrocknung
DE3750847T DE3750847D1 (de) 1987-07-29 1987-07-29 Einrichtung zur Gefriertrocknung.
JP63173852A JP2676374B2 (ja) 1987-07-29 1988-07-14 冷凍乾燥装置
US07/226,536 US4949473A (en) 1987-07-29 1988-07-29 Freeze drying apparatus with additional condensation surface and refrigeration source

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
EP87110955A EP0301117B1 (de) 1987-07-29 1987-07-29 Einrichtung zur Gefriertrocknung

Publications (2)

Publication Number Publication Date
EP0301117A1 EP0301117A1 (de) 1989-02-01
EP0301117B1 true EP0301117B1 (de) 1994-12-07

Family

ID=8197162

Family Applications (1)

Application Number Title Priority Date Filing Date
EP87110955A Expired - Lifetime EP0301117B1 (de) 1987-07-29 1987-07-29 Einrichtung zur Gefriertrocknung

Country Status (5)

Country Link
US (1) US4949473A (es)
EP (1) EP0301117B1 (es)
JP (1) JP2676374B2 (es)
DE (1) DE3750847D1 (es)
ES (1) ES2068809T3 (es)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108469151A (zh) * 2018-02-10 2018-08-31 扬子江药业集团南京海陵药业有限公司 一种注射用磷酸左奥硝唑酯二钠商业化生产的冻干工艺

Families Citing this family (22)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2665338B1 (fr) * 1990-08-02 1994-02-04 Blaizat Claude Procede de concentration, deshydratation de liquide alimentaire ou autre, son dispositif et le produit obtenu.
US5236041A (en) * 1991-07-22 1993-08-17 Hull Corporation Cyclonic vapor flow condenser
US5199187A (en) * 1991-07-31 1993-04-06 Sp Industries Freeze dryer apparatus having an interim condensing system and use thereof
DE4233479C2 (de) * 1991-10-04 1999-09-02 Inst Mikrobiologie Und Biochem Verfahren und Einrichtung zum Gefriertrocknen, insbesondere von Flüssigkeiten mit Mikroorganismen
JPH0735951B2 (ja) * 1991-10-30 1995-04-19 西部瓦斯株式会社 真空乾燥処理装置
US5291751A (en) * 1992-04-21 1994-03-08 Liquid Carbonic Corporation Cryo-mechanical vapor recovery apparatus
US5456084A (en) * 1993-11-01 1995-10-10 The Boc Group, Inc. Cryogenic heat exchange system and freeze dryer
US6122836A (en) * 1998-05-07 2000-09-26 S.P. Industries, Inc., The Virtis Division Freeze drying apparatus and method employing vapor flow monitoring and/or vacuum pressure control
US6220048B1 (en) * 1998-09-21 2001-04-24 Praxair Technology, Inc. Freeze drying with reduced cryogen consumption
EP1144930A1 (en) * 1999-01-05 2001-10-17 Universal Preservation Technologies, Inc. Vacuum control system for foam drying apparatus
WO2005072790A1 (en) * 2004-02-02 2005-08-11 I.M.T. Interface Multigrad Technology Ltd. Device for directional cooling of biological matter
US8528225B2 (en) * 2009-12-11 2013-09-10 Wyssmont Company Inc. Apparatus and method for continuous lyophilization
WO2011078835A1 (en) * 2009-12-22 2011-06-30 Ima Life North America Inc. Monitoring freeze drying with gas measurement on vaccum pump exhaust
CN103123206A (zh) * 2013-03-21 2013-05-29 楚天科技股份有限公司 一种冻干机
EP3004767B1 (en) * 2013-05-29 2017-12-06 GEA Process Engineering A/S Method of providing inline sterile freeze drying of a product in trays accommodated in a trolley, system for carrying out the method, and use of the method
CN103344096A (zh) * 2013-07-18 2013-10-09 上海千山远东制药机械有限公司 冻干机捕水器
CN105509422B (zh) * 2015-12-24 2018-09-25 甘肃银光化学工业集团有限公司 一种真空冷冻干燥系统及采用该系统对含能材料真空冷冻干燥的方法
CN106468501B (zh) * 2016-08-29 2019-12-27 浙江金石生物科技有限公司 一种氮气保护的铁皮石斛冷冻干燥装置及其冷冻干燥方法
DE102016123490A1 (de) * 2016-12-05 2018-06-07 Innovations-Transfer Uphoff Gmbh & Co. Kg Verfahren und Vorrichtung zur Trocknung im Dampfexplosionsverfahren
WO2020201822A2 (en) * 2019-01-27 2020-10-08 Nguyen Vien Lam Convection current freeze drying apparatus and method of operating the same
CN111504003B (zh) * 2020-03-30 2021-06-11 广西农业职业技术学院 一种冷冻干燥方法及其干燥装置
CN113865273B (zh) * 2021-09-01 2023-01-31 广州韩秀科技有限公司 开放式负压低温干燥设备

Family Cites Families (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR784430A (fr) * 1934-04-14 1935-07-22 Installation pour la préparation de produits en poudre sèche
GB552821A (en) * 1941-12-18 1943-04-27 Arthur Sproul Mcfarlane Improvements in and relating to the desiccation of solutions at low temperatures
US2453033A (en) * 1945-03-08 1948-11-02 York Corp Vacuum drying apparatus using a refrigerant system for heating and cooling
US3230633A (en) * 1961-10-27 1966-01-25 Pennsalt Chemicals Corp Freeze drying apparatus and method
DE1196579B (de) * 1962-02-27 1965-07-08 Leybold Hochvakuum Anlagen Verfahren zum Steuern der Trocknungsgut-Heiztemperatur beim Gefriertrocknen, abhaengig vom Partialdruck eines in der Kammer vorhandenen Gases oder Dampfes
DE1196578B (de) * 1962-02-27 1965-07-08 Leybold Hochvakuum Anlagen Gefriertrocknungsverfahren mit Rueckgewinn dabei fluechtiger Bestandteile
US3191395A (en) * 1963-07-31 1965-06-29 Chicago Bridge & Iron Co Apparatus for storing liquefied gas near atmospheric pressure
US3385073A (en) * 1966-10-06 1968-05-28 Cryo Therm Inc Refrigeration system for shipping perishable commodities
FR1586349A (es) * 1968-10-24 1970-02-13
US3648379A (en) * 1970-03-16 1972-03-14 Horton John T Continuous freeze drying system
US4060400A (en) * 1975-08-22 1977-11-29 Henry L. Franke Refrigerated semitrailer truck for long and local deliveries
US4353222A (en) * 1979-07-04 1982-10-12 Kyowa Vacuum Engineering, Ltd. Vacuum apparatus
JPS5728977A (en) * 1980-07-25 1982-02-16 Osaka Gas Co Ltd Vacuum refrigeration drying and apparatus used therefor
DE3107241A1 (de) * 1981-02-26 1982-09-09 Leybold-Heraeus GmbH, 5000 Köln Kondensator fuer trocknungsanlagen
JPS6015867A (ja) * 1983-07-06 1985-01-26 Fujitsu Ltd 磁気記録再生装置

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108469151A (zh) * 2018-02-10 2018-08-31 扬子江药业集团南京海陵药业有限公司 一种注射用磷酸左奥硝唑酯二钠商业化生产的冻干工艺

Also Published As

Publication number Publication date
ES2068809T3 (es) 1995-05-01
EP0301117A1 (de) 1989-02-01
DE3750847D1 (de) 1995-01-19
JP2676374B2 (ja) 1997-11-12
US4949473A (en) 1990-08-21
JPS6449882A (en) 1989-02-27

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