EP1979081A1 - Mesure, contrôle et régulation des mouvements dirigés de produits dans des installations à lit fluidisé ou à couche fluidisée et installations correspondantes - Google Patents

Mesure, contrôle et régulation des mouvements dirigés de produits dans des installations à lit fluidisé ou à couche fluidisée et installations correspondantes

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Publication number
EP1979081A1
EP1979081A1 EP07702954A EP07702954A EP1979081A1 EP 1979081 A1 EP1979081 A1 EP 1979081A1 EP 07702954 A EP07702954 A EP 07702954A EP 07702954 A EP07702954 A EP 07702954A EP 1979081 A1 EP1979081 A1 EP 1979081A1
Authority
EP
European Patent Office
Prior art keywords
product
microwave radiation
microwave
particles
microwave sensor
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.)
Withdrawn
Application number
EP07702954A
Other languages
German (de)
English (en)
Inventor
Jochen A. Dressler
Manfred Struschka
Bernhard Luy
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.)
Glatt GmbH
Original Assignee
Glatt 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
Application filed by Glatt GmbH filed Critical Glatt GmbH
Publication of EP1979081A1 publication Critical patent/EP1979081A1/fr
Withdrawn legal-status Critical Current

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
    • B01J2/16—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by suspending the powder material in a gas, e.g. in fluidised beds or as a falling curtain
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
    • B01J2/006—Coating of the granules without description of the process or the device by which the granules are obtained

Definitions

  • process plant Widely used in the pharmaceutical industry, but also in the food, feed and fine chemical industries, involves the coating of particulate matter in the fluidized bed or spouted bed by suspensions, solutions, powders or melts.
  • a certain amount of these particles by a process gas stream in a vortex or spout system (hereinafter also referred to as process plant) is set in motion and entrained with the gas stream, preferably air as gas, but possibly also nitrogen or other suitable gases or gas mixtures Find use.
  • the process space is delimited within the process plant by one or more distributor plates, which are designed as a gas distributor and allow the process gas flow evenly and / or divided into different zones.
  • Such distributor plates prevent their design from falling through the particles down into the inflow region of the process gas.
  • one or more spray nozzles are located in the region of this inflow base, by means of which the particles are sprayed with the spray medium and granulated or preferably coated, these are generally referred to as "bottom spray.”
  • Such spray nozzles are commercially available in various designs and are described in particular as US Pat One or preferably used as two- or three-fluid nozzles.To obtain particularly uniform coatings on the particles, the particles in the
  • the spray nozzles can also be attached laterally to the process vessel of the vortex or spouted plant or also to certain internals in vortex or spouted bed plants, wherein they are approximately perpendicular to and / or also preferably here can spray in the direction of the product stream. Corresponding conditions can be found in spouted bed apparatuses.
  • the spray rate with which the coating material is applied to the particles to be coated can either be kept constant over the entire course of the process or can also be adapted during the course of the process. It is important in this
  • the bottom spray method (or equivalent methods with side nozzles) can also be used for the granulation of particles.
  • the bottom spray method or equivalent methods with side nozzles
  • particles encompasses all particulate materials or objects that can be fluidized in the fluidized or jet layer (preferred variants are defined below), which can be granulated or coated in fluidized bed systems.
  • the quality of the fluidization in the fluidized or jet layer through viewing window, mounted in the coating container, by camera systems or through the Measurement of the differential pressure at the distributor plate (eg a sieve bottom plate) can be assessed.
  • Viewports have the disadvantage that they allow observation of the movement of the returning particles only from the outside.
  • the observation through viewing windows is only possible with the aid of strong light sources, which depending on the product may also mean a thermal load on the product particles.
  • Observation by camera systems requires, due to the high particle velocity, a sufficiently fast camera system so that the movements of the fluidized particles remain distinguishable.
  • Camera systems as well as viewing windows require a light source. Dust deposits can contaminate and tarnish camera lenses. The view is so limited. Only expensive flushing systems with flushing gases such as compressed air can reduce the formation of deposits.
  • the measurement of the differential pressure is highly dependent on the air distribution and the flow resistance of the inflow base. Particularly in coating processes with more than one riser, the measurement of the differential pressure is limited meaningful.
  • a direct measurement is possible for example by capacitive measurement methods or by measuring the electrical resistance in the riser.
  • these methods are greatly influenced by influences of product moisture or material property.
  • the dielectric constant of the product also changes during the coating process, so that the capacitive measurements take place under changing conditions.
  • the difference in capacitance change in a filled riser compared to an unfilled riser is very small even under ideal conditions.
  • Interference signals for example due to the influence of the test leads, further restrict the applicability of this method.
  • dust deposits or contamination occurring during the process can be added to the measuring electrodes Lead to incorrect measurements.
  • the resistance measurement can also be impaired by the purified and deionized water used, for example, in pharmaceutical production.
  • WO 98/44341 A1 discloses a method for monitoring and / or controlling and regulating a granulation, agglomeration, instantization, coating and drying process in a fluidized bed or a moving bed by determining the product moisture and an apparatus for carrying out the same Known method.
  • the damping of high-frequency waves smaller than 100 MHz or microwaves by means of moisture present in a fluidized bed is determined by means of a sensor (designed as a planar sensor) which is flush with the inside of the outer wall (designed as a planar sensor).
  • the measurement signal is described as essentially only dependent on the moisture content and the product temperature.
  • the relevant resonant frequency is described as referring to the entire fluidized bed, not individual particles.
  • Electronic measurement signal and "product moisture measured offline” are correlated for calibration.
  • Spray coating and / or granulation processes in the fluidized bed or spouted bed permit, and / or a device, monitoring or control and / or an up- or down-scaling of a given vortex or spout system to another possible with different dimensions of the given facility or at least facilitate.
  • the present invention enables the solution of the problems presented and for the first time a direct measurement, monitoring and / or regulation of the fluidization behavior, both qualitatively and quantitatively.
  • a direct measurement, monitoring and / or regulation of the fluidization behavior both qualitatively and quantitatively.
  • for the first time for each corresponding compartment e.g. for each riser, its own measurement and determination and / or a
  • any differently configured process chamber of a fluidized bed system can be equipped with this measuring method, provided that the product flow in this area has a directed movement with a predetermined direction of movement.
  • Qualitative and quantitative statements about the course of the process and control and regulating tasks are then also possible according to the invention in these process chambers. For example, variants with horizontal circulating product flow are described below.
  • the coupling of the microwave radiation is carried out in the outer region of the respective product stream, in particular in the range of one or more guide devices.
  • the or the microwave sensor devices have combined transmitting and receiving units for microwaves, in particular a transmitting and receiving unit per measuring point, in combination, which allows a particularly simple installation and good coordination.
  • a waveguide in particular tubular, eg in the form of approximately or actually round or polygonal tubes
  • per transmitting unit which may consist of customary for this purpose ladders, especially metals or alloys, one (proximal) end respectively several or preferably a transmitting and receiving units (Mikrowellensensorvor- direction (s)), while the other (distal, lying on the side of the measured product flow) end is closed by a microwave radiation sufficiently permeable cover, for example of a plastic material ,
  • microwave sensor device which in particular at least one transmitting and receiving unit for microwave radiation and, if desired, also include a transmitter
  • a microwave sensor device which in particular at least one transmitting and receiving unit for microwave radiation and, if desired, also include a transmitter
  • commercially available devices can be used, as described for example in US 6037783 or EP 0808454.
  • a material used for the examples shown below model for example, the sensor SolidFlow ® from SWR engineering Messtechnik GmbH, D-79424 Auggen, Germany, with the suitable for processing electronic FME.
  • An adaptation to fluidized bed or spouted systems can be achieved for example by suitable dimensioning of the waveguide.
  • the coupling of the microwave radiation is carried out in the product flow to be examined perpendicular or approximately perpendicular to the main direction of the product stream, but it can also be made at any angle.
  • the coupling of the microwave radiation in the range of one or more guide devices (Leiteinbauten), which are provided within the outer wall of the container of the vortex or spout system, made the (supported by the associated process gas flow) support the directed product flow (ie not on the outer wall but via lying within the outer wall further guide devices or in particular their walls or areas of the walls, which are not part of the outer wall), wherein preferably the coupling via one or more waveguide takes place and the one or more distal ends of the waveguide or the one or more microwave sensor devices are mounted in particular such that they have a (as mentioned, preferably within, ie in particular independent of the outer wall of the system or the coating container disposed within the same) wall of the one or more L.
  • a waveguide per microwave sensor device may be provided, but embodiments of the invention are also in which a microwave sensor device alternately supply two or more waveguides with microwave radiation and the reflected microwave radiation can receive, for example by means of a multiplexer device, the alternating and separate connection one of several waveguides allows.
  • the method according to the invention is preferably carried out in such fluidized bed or jet bed systems in which the product flow to be measured, monitored and / or regulated flows against gravity, ie in particular substantially upward, in particular in fluidized bed systems with one or more Wurster tubes or further in spouted beds having one or more Conductors, each in the lower region with spray direction against the action of gravity (ie in particular substantially upward) or laterally with spray direction perpendicular and / or preferably parallel to the product stream one or more single or preferably more, such as two- or three-fluid nozzles for spraying liquids for coating (coating) and / or granulating particles forming the product stream.
  • Particularly preferred is the application of the method for measuring, monitoring and / or regulating the substantially upwardly directed product stream in the bottom spray method (ie where the spray nozzle (s) are provided in the distributor plate area and spray substantially upwards).
  • a process plant in particular here, a Wurster plant with one or more sausage pipes as Leit Roaden.
  • a reverse product flow may take place (from falling, previously spray-coated and / or granulated product particles, for example can be fed back to the product flow near the ground and thus ultimately perform a circular motion).
  • a very preferred embodiment of the invention relates to a method according to the invention, in which the product stream is measured, monitored and / or regulated within one or more sausage pipes within a fluidized bed plant operating on the Wurster principle (also referred to below as Wurster plant).
  • a (at least substantially) horizontally circulating product stream which rotates about a vertical axis of the process plant, can also be subjected to the process according to the invention.
  • the circulation may be excited and maintained, for example, by means of at least one appropriately shaped distributor plate, for example by suitably shaped slots or openings which at least partially impart to the process gas a component of motion parallel to the bottom, such as conidur plates, gill plates or gas distributor plates with overlapping segments or parts, between which columns allow a corresponding directed process gas flow.
  • conidur plates gill plates or gas distributor plates with overlapping segments or parts, between which columns allow a corresponding directed process gas flow.
  • a corresponding process plant according to the invention or a corresponding method in addition to the at least one distributor plate also at least one (openable and closable at the appropriate time) lateral output. Due to this, product which can no longer be treated can be removed laterally due to the centrifugal force during the circular movement.
  • Such a method according to the invention preferably includes that the removal (in particular automatically) is effected or performed and / or terminated upon entry or reaching of a specific property of the product stream or a corresponding resulting measurement signal of the microwave sensor device, for example automatically.
  • the size of such product particles can be in the micrometer to millimeter range, such as from (about) 50 ⁇ m to (about) 25 mm or from (about) 200 ⁇ m to (about) 10 mm.
  • Directed means in particular that the net current of the particles has a certain (eg linear or circular) direction, whereby, for example due to fluidization, gravitation and turbulence, partial deviations may occur - the better the movement of the particles
  • the clearer measurement signals can be obtained by means of the microwave device, and conversely, the clearer and more constant measurement signals are obtained, the smoother the product flow.
  • the measurement conditions can be easily adjusted so that the influence of moisture or the influence of the spraying process is low, in particular not (at least not only) the attenuation is evaluated, but the particle movement by measuring the particles reflected by the particles Microwave radiation, which is evaluated in terms of frequency and amplitude, preferably both parameters, so (at least) also taking into account the frequency change in reflection by the moving particles because of the Doppler effect.
  • the evaluation is frequency-selective, so that it is ensured that only flowing particles are measured and, for example, stationary deposits or even a disturbing influence of a change in humidity are suppressed.
  • the corresponding microwave sensor device can work more or less like a particle counter, which makes it possible to determine a measurement signal for the amount of particles flowing per unit of time.
  • the formation and forwarding of a measuring signal formed in the course of measurement can cause, for example, to a suitably programmed computer (computer, eg PC), for example the display or tabular or graphical representation of a measurement signal or its evaluation or the system control allows, for example, via the transmitter.
  • a suitably programmed computer computer, eg PC
  • the measurement or measurement signal acquisition can be carried out continuously, in pulses or at intervals, wherein different measurement times are possible for the pulses or interval measurements, for example advantageously relatively short measurement times, for example in the range from fractions of a second to a few minutes.
  • this can be done by setting a filter time or sampling time, for example at an evaluation electronics, for example in the range from 0.2 to 200 seconds, in a possible advantageous variant from 1 to 30 Seconds, can lie.
  • a filter time or sampling time for example at an evaluation electronics, for example in the range from 0.2 to 200 seconds, in a possible advantageous variant from 1 to 30 Seconds, can lie.
  • the irradiated microwaves are electromagnetic waves having frequencies of 300 MHz to 300 GHz, for example advantageously 1 to 100 GHz, for example at 24.125 GHz ⁇ 100 MHz.
  • the method according to the invention can also be used to transfer data (data downwards or upscaling), obtained by means of a fluidized bed or jet bed installation of certain dimensions, to installations with smaller or larger dimensions, preferably automatically by means of corresponding data Software and hardware.
  • In process plants selected from vortex and jet bed plants means, in particular, within the vortex or jet bed tank (ie, not in feeding tubes, for example).
  • the quality eg with regard to degree of fluidization, size and / or speed of the particles in the product stream
  • the uniformity of the product stream, and / or the quantity eg with respect to the amount and / or the speed the particles in the product stream
  • the quantity eg with respect to the amount and / or the speed the particles in the product stream
  • the quality of the product stream is particularly preferred because of their simplicity.
  • the "quality” or “quantity” does not refer to the product moisture as such, i. this is not self-characterized.
  • the invention also relates to the use of one or more microwave sensor devices, preferably each with a transmitting and receiving unit and a waveguide, in a method as described above and below.
  • a further embodiment of the invention relates to devices which are suitable or in particular configured for carrying out a method according to the invention, in particular vortex or jet layer systems which are provided with components mentioned above or below for the components used for the method.
  • a device is preferred in particular according to the preceding paragraph, which is characterized in that at least one waveguide for microwaves is provided for coupling in the microwave radiation emitted by the microwave sensor device or devices which penetrates a wall of a guide device located within the process system which is provided at the distal end with a microwave permeable cover, and whose distal end is provided on a side of said wall facing a product flow approximately flush with the intended product flow facing surface of said wall, while the proximal end to which the Microwave sensor device is coupled, is provided on a side facing away from the intended product flow of said wall.
  • a device according to the above paragraph (B) is characterized by comprising two or more of said guiding means and including a microwave sensor device comprising two or more alternately switchable ones of said waveguides, each one of them leads to each one of the located within the device walls of the guide devices.
  • a device according to paragraph (D) 1 is characterized in that the central height adjustment mechanism is firmly connected to the microwave sensor device and the waveguides and via this with the walls of the guide means, so that a common height adjustment of all said components is possible ,
  • each microwave sensor device comprises a transmitting and receiving unit for microwave radiation and each microwave sensor device one of said waveguide is provided. This also allows the separate measurement for each guide.
  • a device according to paragraph (F) characterized in that one or more height adjustment mechanisms are provided therein for the one or more guide devices. This allows e.g. an adjustment of the height of the baffles in favor of an improved product flow.
  • a device according to one of the paragraphs (F) to (H), characterized in that a microwave sensor device is provided with a waveguide for each guide.
  • each microwave sensor device installed in the region of the central height adjustment mechanism of the guide (s) and preferably firmly connected thereto and thus together with one with it and one wall of one of the guide devices connected waveguide itself is height adjustable.
  • a simple height adjustment can be achieved via a height adjustment mechanism and without the need of slots in the wall of the guide.
  • a likewise preferred device according to one of paragraphs (F) or (G) is characterized in that the one or more microwave sensor devices lie outside the outer wall of the process plant and in each case via waveguides which penetrate the outer wall and in each case one wall of a guide device, connected to the interior of the device. This allows eg good accessibility.
  • (M) Very preferably a device according to one of the paragraphs (H) to (L), characterized in that for each guide means a microwave sensor device is provided, each with a waveguide, so that e.g. each product stream can be measured individually.
  • a device according to any one of paragraphs (A) to (M) is very preferred, which is characterized in that it comprises the spray nozzles in the form of one or more single or multi-fluid nozzles in the region of an inflow floor.
  • a device according to one of the paragraphs (A) to (O) is also very preferred, characterized in that it has one or more guide devices in the form of one or more sausage tubes, that is to say a fluidized bed system based on the Wurster principle ,
  • a device according to one of the paragraphs (A) to (P) is very particularly preferred, which has one or more microwave sensor devices and at least one evaluation, which is an evaluation of reflected by the particles of a product stream microwave radiation in frequency and amplitude, preferably frequency-selective , allows.
  • each microwave sensor device is connected via an evaluation electronics and / or or via further components with an evaluation and / or control unit.
  • the invention also relates to a process installation suitable for a method according to the invention or in particular equipped with at least one microwave device, in which at least one boundary selected from the outside wall, distributor plates and / or guide devices located within the process system comprises at least one intended product movement (7) Form of a product stream facing coupling point for radiated from such a microwave sensor device (8) microwave radiation and at least one intended product flow facing coupling point for reflected from particles of such a product stream microwave radiation (ie in particular the one or more input and output points not necessarily in the range of one or more Guide devices inside the process plant, but must be incorporated in the outer wall and / or in the distributor plate, but alternatively and / or supplementary can be introduced in the distributor plate), wherein apart from the position of the coupling and decoupling point otherwise the other features as in paragraph (A) or one or more of paragraphs (B) to (Q) are realized, wherein the process plant preferably for generating a essentially horizontal circular product flow (in particular by means of at least one as described above in the horizontal circulation process
  • At least one waveguide for microwaves which penetrates at least one of said boundaries, which is provided at the distal end with a microwave-permeable cover, and whose distal end adjoins one at a time, is provided in a corresponding process installation for coupling the microwaves to the one or more microwave sensor devices the product flow side of the boundary (s) is provided, while the proximal end to which the microwave sensor device (s) is or is coupled is provided on a side of the boundary (s) sent to the intended product flow.
  • a device may have two or more of said limitations and include a microwave sensor device having two or more alternately connectable waveguides each leading to one of the boundaries located within the device (process plant).
  • each one Microwave device having a transmitting and receiving unit for microwave radiation and each microwave sensor device of one of said waveguide may be provided.
  • the microwave device (s) may be outside the process plant and in each case connected to the interior of the device via waveguides which penetrate the outer wall of the process plant.
  • the spray nozzles are provided in the form of one or more one-component or multi-component nozzles in the region of an inflow base, in particular for bottom-spray methods.
  • At least one evaluation unit may be provided in each case in the above process plants, which enables an evaluation of the microwave radiation reflected by the particles of a product stream with respect to frequency or frequency and amplitude, preferably frequency-selective, in particular taking into account the frequency change of the radiation reflected by particles within the product stream.
  • the invention also relates to a method mentioned above or below, which uses or is carried out in one of the said devices.
  • Fig. 1 Schematic lateral cross section through an exemplary bottom-spray fluidized bed system with (as an example of a guide) Wursterrohr (ie a Wurster plant) and built-in microwave sensor device together with waveguide.
  • Wursterrohr ie a Wurster plant
  • Fig. 2 Schematic cross section (from above) through an exemplary fluidized bed plant according to the bottom spray principle with (as an example of Leit respondeden) three sausage pipes and a corresponding number of connected via waveguide, located outside of the fluidized bed container microwave sensor devices with central height adjustment for the Wursterrohre
  • Fig. 3 Schematic cross section (from above) through an exemplary
  • Fig. 4 Graphical representation of the measured data of an example of uneven fluidization at 40 mm compared to 50 mm distance between the distributor plate and Wursterrohr with good fluidization.
  • Fig. 5 Graphical representation of the measured data for an example of the influence of different amounts of process air on the fluidization behavior in a Wurster tube.
  • Example 1 Inventive Device for a Method According to the Invention
  • a spray nozzle 4 with optional nozzle collar 5 ensures the application of the coating material to the submitted particles, which with the aid of the inflow over the inflow 3 process gas and the guide 6 (exemplified as (also preferred) riser or Wursterrohr) directed product movement. 7 (Product stream).
  • Microwave radiation is coupled by a microwave sensor device 8 (with (preferably one each) transmitting and receiving unit for microwaves and possibly evaluation electronics) directly or preferably via a waveguide 9 in the guide 6.
  • a microwave sensor device 8 with (preferably one each) transmitting and receiving unit for microwaves and possibly evaluation electronics
  • Positions have the upper, the middle or the lower portion of the guide 6 proven, preferably about the middle of the guide 6 can be used as the optimum position.
  • a slot 11 is integrated, by a height adjustment of the guide 6 with rigid mounting of the transmitting and receiving unit 8 and optionally the waveguide 9 with a proximal End 12 and a distal, product flow-facing end 13 (which should be closed with a microwave transparent material) is possible (for example, when using a Wursterrohrs with a diameter of 22.86 cm and a height of 60 cm and a thickness of 3 mm as used in the examples below, a slot 11 in the range of 6.5 to 12.5 cm below the upper edge of a Wurster tube and / or be provided from 23.5 to 29.5 cm below this upper edge).
  • the slot 11 (or the slots in the presence of several) is covered in operation by a suitable cover device 14 around the area penetrated by the waveguide so that no cross-flow through a slot 11 can affect the measurement.
  • the guide 6 can be varied by a height adjustment mechanism 15 (here, for example, as a fixed arms and an annular area around the Wurster tube, within which the Wurster tube can be moved up or down) in their distance from the distributor plate 3.
  • the microwave radiation is reflected by the fluidized solid particles and received by the receiving unit.
  • the evaluation is carried out by means of an integrated and / or separate evaluation electronics, preferably with respect to frequency and amplitude of the reflected signals. Deposits or non-moving particles can be suppressed by a frequency-selective evaluation.
  • the proximal end 12 of the waveguide and thus the microwave sensor device 8 can be advantageously provided outside the outer wall 16 of the process plant and thus be easily accessible, so that the waveguide penetrates the outer wall 16.
  • the cover means that are not penetrated by the waveguides areas of the outer wall 16 to the waveguide and seal, covered holes in the outer wall 16 may be provided (for example, in a Wursterstrom GPCG15 in a height of 170 mm, 385 mm or 555 mm).
  • the microwave sensor devices 8 may each be provided externally analogously as shown in Fig. 1.
  • a central height adjustment mechanism 15 can be provided jointly for all guide devices 6, 9 is the waveguide, with the microwave radiation from and into the transmitting and receiving unit for microwaves of the microwave sensor device 8, which may also include a measuring electronics, in the interior of the guide 6 can be coupled.
  • the spray nozzles 4 are shown here from above.
  • the microwave sensor devices 8 may also be expedient and advantageous to arrange the microwave sensor devices 8 centrally according to FIG. 3, for example, next to and / or above one another in the middle of the process plant 1 - alternatively it can also be provided that the waveguides 9 each individually with only one central microwave sensor device in each case one transmitting and receiving unit are switched on (for example by means of a multiplexer mechanism which enables the connection of only one of a guide 6 coming waveguide 9, so that by means of only one microwave sensor device 8 still individual measurements for the individual by Leit wornen 6 (shown here as Wursterrohre
  • the microwave sensor device (s) 8 and the waveguides 9 can be used together with the microwave sensor device independently of the central height adjustment mechanism 15 (here schematically simplified) ngen 8 shown) or in particular be directly connected to this (in other words, in the latter case, no separate arms ofvolnverstellmechanismus longer necessary, since the waveguide 9 take this function with, while in the first case connecting arms from the central height adjustment mechanism 15 to the baffles 6) and may
  • each guide 6 is preferably a separate microwave sensor device 8 and a waveguide 9 provide, but is also an embodiment as described above with only one microwave sensor device possible, which makes their measurements alternately on the individual waveguide.
  • the measuring signals for the individual guide devices 6 can, if appropriate via evaluation electronics already integrated into the microwave sensor devices 8, be evaluated and visualized individually or jointly after forwarding to them in one or more evaluation units (for example also integrated in the system control).
  • Example 2 Calibration For operation, a microwave sensor device 8 must first preferably be calibrated. On the other hand, since no absolute values or mass flows are needed to assess the fluidization, it may be sufficient to set a microwave sensor device only in terms of its measuring range (ie without calibration), which is another preferred embodiment.
  • a process plant in particular a fluidized-bed plant according to the bottom-spray principle, or its coating container 2, is filled with an intended amount of particles and the plant is operated at the desired process gas rate (s) for a certain time at a particular setting and minimum and maximum values that occur during this process.
  • the signal output of the microwave sensor device 8 supplies raw data values to a downstream (possibly integrated into the microwave sensor device) evaluation electronics.
  • the evaluation electronics converts the raw signals into usable measurement signals which are then further processed, eg calibrated, visualized, stored (for example, by empirical means) directly by means of the evaluation electronics and / or by means of an evaluation and / or control unit which can be integrated in the system control To collect data for up- or down-scaling) and / or for (for example also automatic) control of the system.
  • P or a measuring signal lying in the range of, for example, 25 to 100% of the maximum signal
  • the fluidization comes to a standstill or is it in varies their intensity, results at the Mikrowellensensorvoriquessausga ⁇ g also a modified measurement signal, so that adjustments of the process parameters are possible.
  • the following areas of application can be covered with the aid of microwave sensors, which represents examples of the method according to the invention, wherein for the exemplary data obtained in FIGS. 4 to 6 a fluidized bed system GPCG15 as mentioned in example 1 with a Wurster tube with a diameter of 22, 86 cm and a height of 60 cm and a material thickness of 3 mm and via a corresponding waveguide a microwave sensor device of the type SolidFlow ® (as mentioned above, to which a shunt resistor (470 ⁇ ) with a 16 bit analog / digital converter ( Conrad AD-USB 4, other analog inputs grounded via a 1 k ⁇ resistor) and a connection adapter connected to the output of the SolidFlow ® transmitter FME, using the software supplied with the converter "AD-USB Data Monitor" is used to record the voltage, set the sampling rate of the converter, and record the data the computer to save and read in Excel, and read out via a RS485 to USB interface converter with the SWR software "FME configuration program" the calibration data
  • Example 3 Example of a method according to the invention for monitoring the
  • a separate microwave sensor device 8 is used for each guide 6 (in particular as a Wurster tube). During the fluidized bed process, each delivers a measuring signal. With uniform fluidization of the particles in the region of the product flow for the region of each guide 6, the measurement signals are almost identical and comparable. In plant control, for example, a mean value and the standard deviation of the signals can be calculated. The individual measured value of each microwave sensor device 8 can then be compared with this mean value. If the individual values of one or more devices 8 are below or above the mean value, the process can be interrupted or the plant operator can be informed. It is also possible to define limits for the mean value, which can cause an action to be undershot or exceeded. The standard deviation can also be evaluated from the mean value.
  • the measuring method according to the invention is therefore an important development and can be part of the PAT (Process Analytical Technology) US FDA initiative "Guidance for Industry, PAT - A Framework for innovative Pharmaceutical Development,” Manufacturing, and Quality Assurance; Pharmaceutical cGMPs, September 2004 "are used as a means.
  • Example 4 Determination of a suitable position for a guide-tube device, here using the example of a riser position.
  • the microwave measurement can be used in baffles 6, in particular in Wurster tube, for example, to determine the distance between baffle 6 (e.g., riser) and baffle 3 during operation of a plant.
  • the aim should be to achieve the most uniform possible fluidization at the selected position of the guide.
  • the measurement signal is recorded at the desired amount of fluidizing air for a certain time. If the signal is non-uniform, as shown by way of example in FIG. 4, the position of the guide 6 is changed so far that a uniform signal is achieved.
  • the Ruidmaschine can vary in the process according to the amount of process gas.
  • the measuring method according to the invention it is possible to determine a process gas quantity at which the product flow in the region of the guide device 6 (in particular in the Wurster tube) is uniform.
  • FIG. An experimental example is shown in FIG. Therein, by way of example, 30 kg of cellulose pellets having a diameter in the range from about 850 to about 1000 ⁇ m are fluidized at process gas quantities of 750 m 3 / h and 1000 m 3 / h.
  • the air volume of 750 m 3 / h is not enough to achieve even fluidization (or flow) at the given Wurster tube position, which is necessary for the overall test. If the amount of air is increased to 1000 m 3 / h, results in a more uniform fluidization of the submitted product.
  • volume change experienced which may be the case, for example, when applying large amounts of material.
  • the fluidization behavior of the product also changes during the process and must be tracked.
  • the changed fluidization behavior is recognized and, if necessary, one (in particular automatic) regulation of the process gas quantity.
  • Example 6 Determination of the Minimum Filling Quantity for Process Containers
  • the measuring method according to the invention for determining the minimum permissible product quantity in a process container is illustrated.
  • a plant is filled with as little product as possible. This saves costs at the beginning of the process development and the starting materials, which are often only available in small quantities. Nevertheless, it is important that the product is optimally fluidized in the process chamber. Therefore, there must not be too much product available to the process in the area of the guide, in particular in the riser. For a later transfer of the process data to the pilot or production scale, ideally an optimal fluidization in the sausage pipe is expected and the spraying rate of the spray nozzle is designed accordingly.
  • the microwave measuring technique the minimum permissible filling quantity for a fluidized bed process can be determined.
  • sugar pellets with a diameter of 850-1000 ⁇ m are filled in stages in a 18 "Wurster coating container After each addition of pellets, the product is fluidized for two minutes at an intake air volume of 1000 m 3 / h
  • the bottom plate of the Wurster tube is 50 mm, which shows an increase in the mean value of the measured signal as more pellets are fed in.
  • the Wurster tube fills more and more until a plateau is reached for a quantity of 20 kg or more of pellets consequently a pellet quantity of 20 kg the minimum possible quantity at which scale-up or scale-down calculations can be performed reliably.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
  • Glanulating (AREA)
  • Length-Measuring Devices Using Wave Or Particle Radiation (AREA)

Abstract

L'invention concerne un procédé de mesure, de contrôle et/ou de régulation des mouvements dirigés de produits fluides dans des installations de traitement (1) sélectionnées parmi les installations à lit et à couche fluidisée pendant un procédé de pulvérisation pour le revêtement et/ou la granulation, dans lequel un rayonnement de micro-ondes est émis sans contact sur un ou plusieurs flux de produits à l'aide d'un ou plusieurs dispositifs de capteurs micro-ondes (8), le rayonnement de micro-ondes réfléchi par les particules de chaque flux de produits est reçu et un signal de mesure est élaboré et émis en fonction du rayonnement de micro-ondes reçu afin de caractériser le flux de produits ; l'invention concerne également l'utilisation correspondante de dispositifs de capteurs à micro-ondes (8) et les dispositifs qui en sont équipés (1).
EP07702954A 2006-02-03 2007-01-23 Mesure, contrôle et régulation des mouvements dirigés de produits dans des installations à lit fluidisé ou à couche fluidisée et installations correspondantes Withdrawn EP1979081A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102006005382A DE102006005382A1 (de) 2006-02-03 2006-02-03 Messung, Überwachung und Regelung gerichteter Produktbewegungen in Wirbel- oder Strahlschichtanlagen und geeignete Anlagen
PCT/EP2007/000544 WO2007090515A1 (fr) 2006-02-03 2007-01-23 Mesure, contrôle et régulation des mouvements dirigés de produits dans des installations à lit fluidisé ou à couche fluidisée et installations correspondantes

Publications (1)

Publication Number Publication Date
EP1979081A1 true EP1979081A1 (fr) 2008-10-15

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EP07702954A Withdrawn EP1979081A1 (fr) 2006-02-03 2007-01-23 Mesure, contrôle et régulation des mouvements dirigés de produits dans des installations à lit fluidisé ou à couche fluidisée et installations correspondantes

Country Status (7)

Country Link
US (1) US8187663B2 (fr)
EP (1) EP1979081A1 (fr)
JP (1) JP2009525472A (fr)
CN (1) CN101426568A (fr)
BR (1) BRPI0707486A2 (fr)
DE (1) DE102006005382A1 (fr)
WO (1) WO2007090515A1 (fr)

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CA2654663A1 (fr) * 2006-06-19 2007-12-27 Mcneil-Ppc, Inc. Particules a enrobage enterique contenant un ingredient actif
DE102019207167B3 (de) * 2019-05-16 2020-09-10 Glatt Gesellschaft Mit Beschränkter Haftung Trennvorrichtung

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Also Published As

Publication number Publication date
DE102006005382A1 (de) 2007-08-16
CN101426568A (zh) 2009-05-06
US20090011118A1 (en) 2009-01-08
WO2007090515A1 (fr) 2007-08-16
BRPI0707486A2 (pt) 2011-05-03
JP2009525472A (ja) 2009-07-09
US8187663B2 (en) 2012-05-29

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