EP3839395A1 - Procédé de documentation, de surveillance et/ou de commande d'un processus de lyophilisation dans une installation de lyophilisation - Google Patents

Procédé de documentation, de surveillance et/ou de commande d'un processus de lyophilisation dans une installation de lyophilisation Download PDF

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Publication number
EP3839395A1
EP3839395A1 EP19217089.2A EP19217089A EP3839395A1 EP 3839395 A1 EP3839395 A1 EP 3839395A1 EP 19217089 A EP19217089 A EP 19217089A EP 3839395 A1 EP3839395 A1 EP 3839395A1
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EP
European Patent Office
Prior art keywords
ice
determined
image
freeze
state variable
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
EP19217089.2A
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German (de)
English (en)
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EP3839395B1 (fr
EP3839395C0 (fr
Inventor
Dr. Frank Harms
Michael Umbach
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.)
MARTIN CHRIST GEFRIERTROCKNUNGSANLAGEN GmbH
Original Assignee
MARTIN CHRIST GEFRIERTROCKNUNGSANLAGEN 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.)
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Publication date
Application filed by MARTIN CHRIST GEFRIERTROCKNUNGSANLAGEN GmbH filed Critical MARTIN CHRIST GEFRIERTROCKNUNGSANLAGEN GmbH
Priority to EP19217089.2A priority Critical patent/EP3839395B1/fr
Priority to ES19217089T priority patent/ES2959471T3/es
Publication of EP3839395A1 publication Critical patent/EP3839395A1/fr
Application granted granted Critical
Publication of EP3839395B1 publication Critical patent/EP3839395B1/fr
Publication of EP3839395C0 publication Critical patent/EP3839395C0/fr
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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 invention relates to a method for documenting, monitoring and / or controlling a freeze-drying process in a freeze-drying system.
  • an item to be dried arranged in drying containers, in particular vials is dried in a freeze-drying process.
  • the drying vessels with the items to be dried are arranged in a drying chamber on temperature-controllable shelves and frozen in the drying chamber, for example at atmospheric pressure.
  • a technical vacuum is then created in the drying chamber.
  • a condenser element in particular a cooling pipe or a cooling coil, is arranged in a condenser chamber which is connected to the drying chamber during what is known as primary drying.
  • the liquid contained in the material to be dried sublimes, which is then deposited as ice on the capacitor element.
  • documentation, monitoring and / or control of a freeze drying process can be based on a Product temperature, in particular the temperature of the item to be dried in the area of a sublimation front of the item to be dried during the main drying and / or during post-drying.
  • Temperature sensors are usually used to measure the product temperature.
  • Known temperature sensors are supplied with energy wirelessly or by wire and transmit the measurement signal wirelessly or by wire.
  • These temperature sensors can be arranged in some drying vessels in a drying chamber of the freeze dryer, with which individual temperatures can be measured selectively (and as representative as possible for all drying vessels arranged in the drying chamber) in these drying vessels. In the drying vessels, however, the temperature sensors may already falsify the process conditions compared to the drying vessels in which no temperature sensor is arranged. Due to the presence of the sensor, it can e.g. B. in the drying vessel to a changed crystallization behavior.
  • the temperature sensors measure the temperature in the drying vessel at a specific measuring point, which, depending on the arrangement of the temperature sensor and / or the progress of the drying process, can be arranged in the area of the frozen items to be dried or in the area of an already dried so-called cake of the items to be dried, whereby the temperature sensor does not accurately measure the temperature at the sublimation front. If the temperature sensor is used in the drying vessel, however, it must be ensured that the measured temperature is representative of the drying process, which is only possible to a limited extent. The reason for this is that temperatures of the items to be dried in different drying vessels of a batch can be different, the temperature, for example, being dependent on whether a drying vessel is arranged further inside or further outside in a drying chamber of the freeze dryer.
  • the patent literature describes a pressure-based determination of a product temperature during a freeze-drying process and the use of the product temperature determined in this way for process control in a freeze dryer, for example in the publications DE 1 038 988 B , EP 2 156 124 B1 , EP 1 903 291 A1 and US 6,971,187 B1 described.
  • a residual moisture content of the items to be dried in a drying vessel is determined based on the mass of the drying vessel with the items to be dried therein, this mass being recorded during the freeze-drying process by a load cell located in the drying chamber.
  • the determined mass and / or the sublimated moisture that can be determined from the change in mass and / or the remaining residual moisture, which can / can be determined quasi-continuously, are then taken into account by the process control of the freeze-drying process.
  • Corresponding load cells are sold by the applicant under the label "LyoBalance".
  • the invention is based on the object of proposing an alternative or cumulative method for the documentation, monitoring and / or control of a freeze-drying process in a freeze-drying system.
  • the invention proposes a method for documenting, monitoring and / or controlling a freeze-drying process in a freeze-drying system.
  • the freeze-drying system has a condenser chamber in which a condenser element, in particular a cooling pipe or a cooling coil, is arranged.
  • a condenser element in particular a cooling pipe or a cooling coil.
  • moisture accumulates on the capacitor element Shape of ice. This moisture is the moisture that has been extracted from the goods to be dried in a sublimation process in the freeze-drying process.
  • the freeze-drying process and, in particular, the primary drying is carried out by suitable process control, in particular the design of the temperature and pressure conditions and the creation of a connection between the condenser chamber and the drying chamber.
  • suitable process control in particular the design of the temperature and pressure conditions and the creation of a connection between the condenser chamber and the drying chamber.
  • an image of the ice is recorded with a camera.
  • the invention here comprises embodiments in which the camera captures an image (of a part) of the capacitor element, with which the camera then also captures ice deposited on the capacitor element, which can then be subjected to further analysis.
  • the camera it is also possible (alternatively or cumulatively) for the camera to take an image of another point in the condenser chamber where ice is deposited during the drying phase, so that this ice can then be subjected to further analysis.
  • ice is deposited on the condenser element or elsewhere in the condenser chamber during the freeze-drying process, this ice is also documented with the recorded image. Subsequently, according to the invention, an automatic image evaluation is carried out with regard to the recorded image of the ice.
  • the automatic image evaluation is carried out with the aim of determining an ice condition variable of the ice in the recorded image.
  • the invention also includes embodiments in which only one image is recorded in the method, according to the invention, several images are preferably recorded at different times, which can be done at short time intervals to generate a film or by means of individual, time-spaced images . It is possible, for example, for an image to be recorded in each case after fixed predetermined time intervals, in particular after a time interval in the range from 10 to 50 minutes or from 20 to 40 minutes. It is also possible for the image to be recorded alternatively or additionally at specific process times, for example at the start or end of freeze-drying, with a change in a process parameter, in particular one Temperature or a pressure (which can be the pressure in the drying chamber and / or the condenser chamber), or with a change in the temperature control of the shelves.
  • a process parameter in particular one Temperature or a pressure (which can be the pressure in the drying chamber and / or the condenser chamber), or with a change in the temperature control of the shelves.
  • freeze-drying process it is also possible for the freeze-drying process to be monitored using the process parameters by means of a control unit. If the process control signals that unexpected process variables occur, which for example indicate a possible error in the course of the process, this can trigger the recording of at least one image and the automatic image evaluation.
  • a viewing window is provided on the condenser chamber anyway, through which an operator can inspect the cooling coil (or another point in the condenser chamber where ice can deposit), and below
  • a camera is also present, by means of which an image of the interior of the condenser chamber or the cooling coil (and the ice formed) is recorded through the viewing window.
  • the present invention also encompasses embodiments in which not only one type of the aforementioned ice state variables is determined, but at least two different ice state variables are determined.
  • the recorded image is based on an illumination of the ice with daylight, which in particular reaches the condenser chamber via a sight glass. It is also possible, however, for the ice to be illuminated via a light source that can be arranged in the condenser chamber or that sends light into the interior of the condenser chamber through the sight glass of the condenser chamber.
  • the light source forms a structural unit with the camera. The light source can be permanently effective or can only be activated in the temporal vicinity of the recording of an image by the camera.
  • the light source can generate light in any spectral range, in particular light in the visible range, light in the IR range, light in the ultraviolet range, light in the invisible range or light both in the invisible range and in the visible range. It is also possible for the image to be evaluated or recorded using (optical) filters.
  • the capacitor element can be recorded using two cameras with two different recording directions.
  • a reference point, a reference grid or any reference curve can be projected onto the surface of the capacitor element (possibly with ice deposited on it) and by means of at least one camera that preferably records an image in a direction that deviates from the projection direction, a shift of the reference point, the grid and the like can be detected as the thickness of the ice increases.
  • an image is generated using a light section technique and the known evaluation methods based on this are used.
  • the extent determined by means of the automatic image evaluation is a length. This can be, for example, the length over which the ice extends on the capacitor element or in the capacitor chamber. It is possible here for the length of the ice to extend in a direction vertical to a surface of the Capacitor element or a surface in the capacitor chamber on which ice is deposited is determined. However, the length is preferably a layer thickness of the ice or a radius or a diameter of the outer contour of the ice on a cooling tube. For the design of the capacitor element as a cooling tube, the length of the extent of the ice is thus determined in a radial direction of the cooling tube.
  • a length measuring scale it is possible for a length measuring scale to be attached to the capacitor element, which scale extends vertically to a surface of the capacitor element or vertically to a surface in the capacitor chamber on which ice is deposited.
  • the length measuring scale thus extends in the radial direction. If ice is deposited on the surface, part of the length measuring scale is covered by this ice. The image evaluation can then be used to determine on the length measuring scale how large the length of the cover of the length measuring scale is.
  • the length measuring scale is a kind of ruler.
  • the determined extent is an area. If, for example, the camera records an image in the manner of a projection of a cooling tube with ice deposited thereon, ideally with a constant layer thickness, this projection results in a rectangular area which is covered by the ice. If this area is evaluated, the volume of the ice can be determined from the determined area via a map, the geometric relationship between this area and the hollow-cylinder-shaped deposit of the ice or any functional dependency.
  • the mass of the ice can be different for different structures of the ice with the same extent of the ice or the same volume of the ice: If the ice is solid, for example as glass ice, the same volume of ice may have a greater mass than when the ice has a crystalline structure with the inclusion of a gas or of cavities with a (technical) vacuum therein and / or when the ice is needle-shaped or otherwise with a lower density, for example as structured ice.
  • the mass of the ice is determined from the determined extent of the ice, taking into account the determined contour of the ice and / or the determined structure of the ice.
  • An evaluation of whether a process sequence is correct and / or a desired process state has been achieved can, for example, by using absolute values for the extent of the ice, for contour values of the ice and / or for structural values of the ice (for example by comparing the determined values with Target threshold values, target contour courses or target structures).
  • a desired target state it is also entirely possible for a desired target state to be achieved in the course of the process for different processes actually carried out for different extensions of the ice, different contours of the ice or different structures of the ice.
  • the invention proposes that the multiple images and / or the determined ice condition variables not be evaluated in absolute terms, but rather a change in the ice condition variable over time is determined from the several recorded images.
  • the appearance of the ice and the capacitor element arranged below it or of a component of the capacitor chamber can in principle be evaluated in the image evaluation.
  • a marking element and / or a reflection element is attached to the capacitor element or in the capacitor chamber.
  • ice is (also) deposited on the marking element and / or reflection element.
  • a process can then be achieved through the covering of the marking element and / or reflection element by the ice resulting change in the image can be evaluated.
  • a marking element without ice deposited on it can be easily identifiable with an assigned image value, in particular a defined gray level or a color. If the marking element is covered by ice, the marking element must be taken up through the ice. Depending on the thickness of the ice and / or the color of the ice (i.e. the structure of the ice), the ice is then more or less transparent or translucent. From the change in the image value, i.e. a change in the gray level of the image point and / or a change in the color of the image point, conclusions can then be drawn about the extent of the ice, the contour of the ice or the structure of the ice.
  • a reflection element can be attached to the capacitor element or in the capacitor chamber, which can reflect light from a light source, a laser and the like, for example.
  • the reflected light has to reach the reflection element through the ice and be reflected therefrom and reach the camera again through the ice.
  • conclusions can then be drawn about the extent of the ice, the contour of the ice and / or the structure of the ice on the basis of the light recorded by the camera at the image point.
  • a contour course of the ice can be determined in the area of the outer or lateral surface thereof. This can be done using common methods, for example by changing the image values when the outer contour of the ice is reached. It is also possible to use a differential method to determine a contour profile, in which a known image of the capacitor element or the capacitor chamber without ice is "subtracted" from the image of the capacitor element or the capacitor chamber with the ice.
  • a variation of image values of image points of the recorded image in the area of the identified ice is evaluated.
  • This proposal is based on the knowledge that, in the ideal case of a glass ice, the image values in the area of the ice show little or no variation, while an irregular ice or structured ice formed by individual ice particles can be recognized on the basis of a greater variation in image values. In this way, conclusions can be drawn about the structure of the ice from the variation in the image values.
  • the result of the evaluation can be used, i.e. what the image of the ice recorded by the camera and / or the determined ice state variable and / or the determined mass of the ice is used for: For a first suggestion, the determined result is saved for process documentation.
  • the result is also possible for the result to be displayed on a display device for an operator of the freeze-drying system.
  • a freeze-drying process can be terminated on the basis of the result. Is for example after a predetermined period of time a drying phase, the determined extent of the ice below a threshold value, it can be concluded that the sublimation did not take place as desired, which means that the freeze-drying process can be terminated. It is also possible for the result to be taken into account in order to determine the end of a drying phase (possibly taking into account further supplementary process parameters or measured variables).
  • an ice state variable is determined before the start of the freeze-drying process. If the determined ice state variable indicates that there is still ice on the condenser element or in the condenser chamber from a previous freeze-drying process before the start of the freeze-drying process, an optical or acoustic warning can be generated for the operator, an error entry can be made or the execution of the freeze-drying process can be prevented.
  • This embodiment of the invention is useful when it is necessary to ensure that no ice is present at the start of the freeze-drying process so that, for example, defined process conditions are present at the start of the freeze-drying process.
  • an ice condition variable can be determined during a defrosting process of the capacitor element or the capacitor chamber. For example, it can be determined whether the ice is damp, from which it can be concluded that the defrosting process is about to begin.
  • the change in volume of the ice on the capacitor element or in the capacitor chamber during the draining process can also be monitored by means of a suitable ice condition variable, in particular the extent. It is possible that the change in the extent or the volume of the ice on the capacitor element or in the capacitor chamber is used to determine or approximate when or when the capacitor element or the capacitor chamber is completely defrosted. In this case, a message can be given to the user or an entry can be made in process documentation. It is also possible in this case for a defrosting process to be ended automatically on the basis of the determined ice state variable.
  • the ice condition variable it is possible for the ice condition variable to be determined directly from the recorded image or for a calculation of the same to be determined using a functional dependency, a characteristic diagram, a proportionality constant and the like.
  • a layer thickness or a diameter of the ice can be determined from the image.
  • the mass of the deposited ice and thus the sublimated liquid can then be determined via the dependency or the characteristic field from the determined layer thickness or the diameter of the ice.
  • the dependency takes into account the influence of several parameters.
  • the influence of the color or the variability of the color of the ice in the image can be taken into account in the dependency, so that a greater mass of the deposited ice is determined for the same layer thickness for glass ice than for structural ice.
  • a calibration method is carried out in which an actual ice state variable is specified or determined in (at least) one calibration process.
  • a predetermined mass of ice with a predetermined volume (layer thickness, diameter) and a predetermined color of the ice is deposited on a capacitor element in the calibration process, with the mass, the volume, the layer thickness, the diameter and / or the color can be the known or determined actual ice state variable.
  • An image is then recorded and a calibration variable for the ice condition is determined from the image, as has been explained above.
  • a dependency or a characteristic diagram it can then be stored that the determined at least one calibration ice condition variable (layer thickness, diameter, color of the ice) correlates with the a priori known or determined mass of the ice.
  • a variation of the predetermined mass of the ice and / or further ice state variables such as the volume or the generated color of the ice can then take place, with which the dependency or the characteristic diagram can be further completed.
  • one freeze-drying process ice state variable can be determined in a freeze-drying process.
  • an actual ice state variable for example the mass of the ice deposited in the freeze-drying process, can then be determined from the freeze-drying process ice state variable.
  • Fig. 1 shows, in a highly schematic and exemplary manner, a capacitor element 1, which is designed in particular as a cooling coil and is shown here in the region of a section of the same in the form of a cooling tube 2.
  • Fig. 1 shows the capacitor element 1 during a first drying phase of the freeze-drying process after ice 3 has already deposited on the capacitor element 1 as a result of the sublimation that has taken place.
  • a length measuring scale 4, in particular a ruler 5, is held on the capacitor element 1.
  • the length measuring scale 4 extends vertically to a surface 6 of the capacitor element 1.
  • the ruler 5 extends radially to the cooling tube 2.
  • the ruler 5 can be held on the cooling tube 2, for example, by a clamp encompassing the cooling tube 2 be.
  • a camera 14 is used to generate an image 9 of the capacitor element 1 with the ice 3, which is viewed from the same direction as shown in Fig. 1 , that is, when the capacitor element 1 is designed as a cooling tube 2, it is recorded with a viewing direction in the radial direction. Assuming that a contour 8 of the ice 3 is straight, the recorded image 9 shows a rectangular extension of the ice 3 between the upper contour 8a and the lower contour 8b.
  • Fig. 2 shows schematically a section of a condenser chamber 10 of a condenser 11 of a freeze-drying system.
  • the condenser element 1 here the cooling tube 2
  • the capacitor 11 has a housing 12 which delimits the capacitor chamber 10.
  • the housing 12 has a transparent sight glass or viewing window 13 through which it is possible to inspect the condenser chamber 10 and to assess the condenser element 1, possibly with the ice 3.
  • a camera 14 is arranged outside the housing 12.
  • the camera 14 is preferably designed as a CCD camera.
  • the camera 14 records, for example, an image 9 of the capacitor element 1 with the ice 3 possibly deposited thereon in a recording direction 15 which is arranged radially to the cooling tube 2.
  • Figs. 3 and 4 show different contours 8 of the ice 3: According to Fig. 3 the contour 8 is straight. If such a straight contour is recognized by an automatic image evaluation, it can be concluded, for example, that it is glass ice or an ice with a structure of a specific type. In contrast, the contour 8 is in accordance with Fig. 4 non-uniform with a multitude of relative maxima and minima, inflection points and a varying slope. If such a contour 8 is recognized by means of the automatic image evaluation, it can be concluded that the structural ice or ice with a structure of another specific type is present.
  • Fig. 7 shows an image area 16 in which there is a greater variation in the image values at the image points. For the sake of simplification, continuous partial areas with two different image values are shown in the image area 16. But it can also be different Fig. 7 result in a change in the image values with a large number of different continuously varying image values and the boundaries of a partial area with a certain image value range can also be gradual. If the automatic image evaluation detects a large variation in the image values in the image area 16, it can be concluded that it may be structural ice. On the other hand, conclusions can also be drawn about the structure of the ice from the size and / or contour of partial areas 17 with a predetermined image value range.
  • Figures 8 and 9 show an image area 16 in the area of a marking element 18 which is attached to the surface 6 of the capacitor element 1.
  • the marking element 18 is, for example, a single or multi-colored marking. It is also possible for a reflection element 19 to be attached to the surface of the capacitor element 1.
  • a contrast or a change in the image values in the area of the marking element 18 or reflection element 19 compared to the area away from the marking element 18 or the reflection element 19 is greater than this according to FIG Fig. 9 the case is. From this, conclusions can be drawn about the extent of the ice and / or the structure of the ice. For example, according to Fig. 8 the layer thickness 7 of the ice may be smaller than this according to Fig. 9 the case is. It is also possible that it is according to the ice Fig. 8 is glass ice, while according to Fig. 9 Structured ice is present.
  • Fig. 10 shows a partial section of the capacitor chamber 10 with the capacitor element 1 and ice 3 deposited thereon.
  • the length measuring scale 4 is not attached to the capacitor element 1, but it is arranged at any other point in the capacitor chamber 10 at which is on a surface Ice forms.
  • the length measuring scale 4 is preferably arranged vertically to the surface on which the ice forms.
  • the length measuring scale 4 is more or less covered, which can be detected on the basis of the image evaluation.
  • a marking element 18 or a reflection element 19 insert which is arranged here at a distance from the capacitor element 1 at a point at which ice can deposit on the marking element 18 or the reflection element 19. Since a greater layer thickness of the ice forms on the surface of the marking element 18 or the reflection element 19 with increasing sublimation, the optical appearance of the marking element 18 or the reflection element 19 changes in the recorded image 9, from which the ice condition size can then be determined by means of the image evaluation .
  • the marking element 18, the reflection element 19 or the length measuring scale 4 is not attached to a cooled element such as the capacitor element 1.
  • the methods known per se for this purpose can be used for the image evaluation within the scope of the invention.
  • the automatic image evaluation can include methods of “image recognition” and / or “image understanding”.
  • an image preparation can take place, which can have point operations, local operations and global operations.
  • a point operation an expansion of the color or gray scale, a binarization or threshold value formation, a color transformation, a background subtraction, a masking and / or a geometric transformation can take place.
  • a linear convolution, a mean value operator or low-pass filter, a Laplace operator or high-pass filter, an increase in edges in a preferred direction, a Sobel operator, a gradient and the like can be used as local operations.
  • Edge-oriented segmentation can also be used, in which edge detection, edge thinning or skeletonization or edge tracking takes place. Furthermore, a model-dependent segmentation can take place with a matching (comparing the image with a pattern) or a Hough transform. It is possible for geometric features to be obtained by means of the automatic image evaluation, in particular an area, a circumference, a length and / or a width. Furthermore, a compactness or roundness can be determined, for which purpose the circumference of an identified object can be used.
  • a convex envelope can be determined as a rectangle or an orthogonal envelope that allows steps from rectangular angles or the determination of a convex core.
  • Pattern recognition with a numerical classification (in particular a linear classification, a distance classification, a statistical classification, a context-dependent classification, a discrete relaxation, a continuous relaxation) can be used. Furthermore, a three-dimensional image interpretation with the generation of a 21 ⁇ 2 D sketch is possible Edge marks or node marks or a Walz algorithm can be used to determine the contour.
  • the condenser chamber prefferably be cleaned before or after a freeze-drying process in order to ensure sterile conditions.
  • H 2 O 2 can be applied to the condenser chamber for cleaning purposes. It is counterproductive here if there is still ice on the capacitor element or if there is residual moisture on the capacitor element. On the basis of the recording of an image by the camera, it can be detected whether there is still ice on the capacitor element or whether it is still damp, which means that the cleaning process cannot be permitted or a corresponding warning can be given.
  • a length measuring scale 4 a marking element 18 or a reflection element is connected via a thermal decoupling element to the surface on which ice is deposited and on which the extent of the ice is to be recorded.
  • a dependency of the determined ice state variable, which is determined from the image recorded by the camera of the ice, on the progress of the sublimation, for example the mass of the sublimed liquid or the mass of the deposited ice, or a map is determined by taking into account the residual moisture, the change in the mass of the drying material, which is determined by means of load cells according to DE 102012 007 422 A1 have been determined.

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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)
EP19217089.2A 2019-12-17 2019-12-17 Procédé de documentation, de surveillance et/ou de commande d'un processus de lyophilisation dans une installation de lyophilisation Active EP3839395B1 (fr)

Priority Applications (2)

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EP19217089.2A EP3839395B1 (fr) 2019-12-17 2019-12-17 Procédé de documentation, de surveillance et/ou de commande d'un processus de lyophilisation dans une installation de lyophilisation
ES19217089T ES2959471T3 (es) 2019-12-17 2019-12-17 Procedimiento para la documentación, monitorización y/o control de un proceso de liofilización en una instalación de liofilización

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EP19217089.2A EP3839395B1 (fr) 2019-12-17 2019-12-17 Procédé de documentation, de surveillance et/ou de commande d'un processus de lyophilisation dans une installation de lyophilisation

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EP3839395A1 true EP3839395A1 (fr) 2021-06-23
EP3839395B1 EP3839395B1 (fr) 2023-07-19
EP3839395C0 EP3839395C0 (fr) 2023-07-19

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DE102016100163A1 (de) 2016-01-05 2017-07-06 Martin Christ Gefriertrocknungsanlagen Gmbh Gefriertrockner-Steuereinrichtung, Verfahren zum Betrieb derselben, Gefriertrockner und Gefriertrocknungsanlage
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WO2004029529A1 (fr) * 2002-09-18 2004-04-08 Sueverkruep Richard Procede de production d'une preparation d'une matiere pharmaceutique sous forme de lyophilisat et installation adaptee a cet effet
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EP2156124B1 (fr) 2006-09-19 2012-04-25 Telstar Technologies, S.L. Procédé de commande de processus de lyophilisation
DE102012007422A1 (de) 2012-04-16 2013-10-17 Martin Christ Gefriertrocknungsanlagen Gmbh Verfahren zur Gefriertrocknung von Substanzen und Anlage zur Durchführung dieses Verfahrens
WO2015189655A1 (fr) * 2014-06-10 2015-12-17 Alberio Marco Système de surveillance de la quantité de solvant extrait pendant l'étape de lyophilisation de substances
CN205209079U (zh) * 2015-11-05 2016-05-04 江苏兴野食品有限公司 一种冻干机
DE102016100163A1 (de) 2016-01-05 2017-07-06 Martin Christ Gefriertrocknungsanlagen Gmbh Gefriertrockner-Steuereinrichtung, Verfahren zum Betrieb derselben, Gefriertrockner und Gefriertrocknungsanlage
CN110057103A (zh) * 2019-05-30 2019-07-26 刘赟 空气换热装置、液囊式翅片蒸发器、空气能热泵及热水器

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