EP3784004A1 - Commande d'applicateur à micro-ondes - Google Patents

Commande d'applicateur à micro-ondes Download PDF

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Publication number
EP3784004A1
EP3784004A1 EP19192286.3A EP19192286A EP3784004A1 EP 3784004 A1 EP3784004 A1 EP 3784004A1 EP 19192286 A EP19192286 A EP 19192286A EP 3784004 A1 EP3784004 A1 EP 3784004A1
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EP
European Patent Office
Prior art keywords
microwave
power
product
amount
controller
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
EP19192286.3A
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German (de)
English (en)
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EP3784004B1 (fr
EP3784004C0 (fr
Inventor
Carlo Groffils
Vincent GOOVAERTS
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Meam BV
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Meam bvba
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Application granted granted Critical
Publication of EP3784004B1 publication Critical patent/EP3784004B1/fr
Publication of EP3784004C0 publication Critical patent/EP3784004C0/fr
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    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B6/00—Heating by electric, magnetic or electromagnetic fields
    • H05B6/64—Heating using microwaves
    • H05B6/70—Feed lines
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B6/00—Heating by electric, magnetic or electromagnetic fields
    • H05B6/64—Heating using microwaves
    • H05B6/80—Apparatus for specific applications
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B2206/00—Aspects relating to heating by electric, magnetic, or electromagnetic fields covered by group H05B6/00
    • H05B2206/04—Heating using microwaves
    • H05B2206/045—Microwave disinfection, sterilization, destruction of waste...
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B2206/00—Aspects relating to heating by electric, magnetic, or electromagnetic fields covered by group H05B6/00
    • H05B2206/04—Heating using microwaves
    • H05B2206/046—Microwave drying of wood, ink, food, ceramic, sintering of ceramic, clothes, hair

Definitions

  • the present invention is in the field of microwave applicators, and in particular in the field of methods and devices for controlling microwave applicators.
  • Microwave systems are used for a variety of purposes including heating, drying, and assisting chemical reactions.
  • the following prior art is made of record:
  • the present methods and systems address at least these needs.
  • a method for applying a microwave treatment to a product comprising the steps: a) providing a microwave system comprising a microwave applicator, an imaging device, a controller, and a microwave generator; b) placing the product in the microwave applicator; c) generating microwaves by means of the microwave generator at a pre-determined generated microwave power; d) directing the microwaves to the product in the microwave applicator; e) subjecting the product to the microwaves at a pre-determined applied microwave power; f) capturing, by means of the imaging device, image data indicative of a temperature distribution of the product; g) controlling, by means of the controller and based on the image data, the applied microwave power to the product.
  • the imaging device comprises an infrared camera.
  • step b) comprises the following sub-steps: b1) providing one or more positioning blocks in the microwave applicator; and, b2) placing the product on the one or more positioning blocks.
  • step g) comprises the steps: g1) determining, by the controller and based on the image data captured by the image device, an amount of excess generated microwave power; and, g2) directing, by means of a circulator, the excess generated microwave power to a dummy load.
  • step g) is followed by step h) which comprises the following steps: h1) measuring an amount of incident power by means of a power meter; h2) measuring an amount of reflected power by means of a power meter; h3) determining an amount of absorbed microwave power by subtracting the amount of incident power and the amount of reflected power; h4) either using the amount of absorbed microwave power as an approximation of the amount of microwave power that was absorbed by the product; or, calculating an amount of cavity losses, and calculating the amount of microwave power that was absorbed by the product by subtracting the amount of cavity losses from the amount of absorbed microwave power.
  • the product is a liquid product, and wherein the method further comprises the step of stirring the product.
  • step f) further comprises the step of determining a temperature distribution in the product based on the image data, and wherein in step g), the applied microwave power to the product is further controlled based on a maximum, average, or minimum value of the temperature distribution in the product.
  • the applied microwave power is further controlled by means of a power limiter that limits the maximum applied microwave power.
  • a microwave system for subjecting a product to a microwave treatment, the system comprising a microwave applicator, an imaging device, a controller, and a microwave generator; wherein the controller is operationally coupled with the microwave applicator, the imaging device, and the microwave generator; wherein the microwave generator is arranged to generate microwaves at a pre-determined power; wherein the system is arranged to subject the product to the microwaves; wherein the imaging device is arranged to capture image data indicative of a temperature distribution in the product; and, wherein the controller is arranged to adapt the power at which the microwaves are applied to the product based on the captured image data.
  • the imaging device comprises an infrared camera.
  • the system further comprises one or more positioning blocks for supporting the product.
  • the system further comprises a circulator and a dummy load, wherein the controller is further configured to determine an amount of excess generated microwave power based on the image data captured by the image device; and wherein the circulator is configured for directing the excess generated microwave power to a dummy load.
  • the system further comprises a power meter for measuring an amount of incident power and a power meter for measuring an amount of reflected power, wherein the controller is configured to determine an amount of absorbed microwave power by subtracting the amount of incident power and the amount of reflected power.
  • the controller is further configured for calculating an amount of cavity losses, and calculating the amount of microwave power that was absorbed by the product by subtracting the amount of cavity losses from the amount of absorbed microwave power.
  • system further comprises a stirrer and/or a power limiter.
  • 100 - microwave system 200 - microwave applicator (also called cavity); 201 to 207 - openings in the cavity (200); 2071 - PTFE sheet; 210 - microwave applicator door; 220 - infrared camera; 230 - vacuum suction line; 240 - pressure gauge; 250 - vacuum sensor; 260 - pressure feed; 270 - vacuum bleed line; 280 - vacuum pump; 285 - integrated water pump and chiller; 290 - product discharge and collection device; 291 - upper valve; 292 - lower valve; 300 - controller; 400 - microwave generator; 450 - wave guide; 500 - circulator; 520 - wave guide; 540 - coupler; 550 - power meter; 560 - sub-tuner module; 600 - dummy load; 700 - multi-purpose module; 800 - weighing scale; 1000 ultrasound aid.
  • a measurable value such as a parameter, an amount, a time period, and the like
  • a measurable value such as a parameter, an amount, a time period, and the like
  • a method for applying a microwave treatment to a product comprising a) the step of providing a microwave system comprising a microwave applicator, an imaging device, a controller, and a microwave generator.
  • a microwave applicator which is also called a cavity.
  • microwaves are generated by means of the microwave generator at a pre-determined generated microwave power.
  • microwaves are directed to the product in the microwave applicator.
  • the product is subjected to the microwaves at a pre-determined applied microwave power.
  • an imaging device captures image data indicative of a temperature distribution of the product.
  • the controller controls the applied microwave power to the product based on the image data.
  • the method further employs one or more wave guides, a circulator, a coupler, a power meter, a sub-tuner module, a multi-purpose module, and/or a weighing scale.
  • the method further employs one or more of the following ancillary components: a microwave applicator door, an infrared camera, a vacuum suction line, a pressure gauge, a vacuum sensor, a pressure feed, a vacuum bleed line, a vacuum pump, an integrated water pump and chiller, and/or a product discharge and collection device.
  • ancillary components a microwave applicator door, an infrared camera, a vacuum suction line, a pressure gauge, a vacuum sensor, a pressure feed, a vacuum bleed line, a vacuum pump, an integrated water pump and chiller, and/or a product discharge and collection device.
  • the microwave applicator door can be closed by means of a plurality of butterfly nuts.
  • the method employs a discharge and collection device as described herein.
  • the microwave system is further equipped with one or more pressure regulating devices, preferably one or more pressure regulating device selected from the list comprising a vacuum suction line, pressure gauge, vacuum sensor, pressure feed, vacuum bleed line, and a vacuum pump.
  • one or more pressure regulating devices selected from the list comprising a vacuum suction line, pressure gauge, vacuum sensor, pressure feed, vacuum bleed line, and a vacuum pump.
  • the system is used in a method for drying an object.
  • the door is closable by means of a plurality of bolts, for example between 5 and 15 bolts.
  • the bolts are made of aluminium.
  • the method is performed in a well-ventilated place.
  • the method is applied in an atmosphere having a temperature below 30°C.
  • the method involves the step of closing and securing the cavity door during operation of the microwave system.
  • the method comprises the step of providing cooling water.
  • the cooling water is used in a dummy load or isolator to absorb mismatched (i.e. reflected) microwaves, thereby preventing them from bouncing back to the magnetron.
  • the cooling water is used for cooling the magnetron.
  • Using cooling water both in the isolator and for cooling the magnetron significantly improves the operation of the microwave applicator and the life expectancy of the electronics inside.
  • the microwave (MW) unit is preferably not operated without a supply of cooling water at the correct temperature of, for example, between 10°C and 30°C. This can be enforced by requiring, for example, that the magnetron will not start if the water flow is too low or if the cooling water is too hot.
  • the cooling water is circulated by a water pump that is integrated with a chiller.
  • the water pump and chiller are comprised in an integrated water pump and chiller.
  • the total cooling water volume of the microwave system is between 5 and 15 liters, for example 10 liters.
  • the level of the water is preferably between the maximum and minimum lines in the level meter of the cooling unit.
  • the water used is preferably solids-free and preferably does not contain any organic contaminants, such as, oils. Distilled water or potable water is suitable for this purpose.
  • the method is used for drying products and the method comprises the step of checking whether or not the product is sufficiently dry by performing the following steps: a) ascertain the weight of the collector tank with its vacuum seal (tare); b) ascertain the initial moisture and weight of the product (measured by, e.g., IR scale); c) calculate the theoretical weight loss based on the initial moisture content and the desired end moisture content; and d) check the dryness of the material by weighing.
  • the method is used for tempering or softening frozen foodstuffs, which comprises cooling the surface of the frozen foodstuffs with non-polar non-ionic cooling media during microwave radiation.
  • the temperature at the surface may be as low as -40 °C to prevent surface thawing.
  • the coolant may be carbon dioxide, nitrogen or argon.
  • the method comprises applying microwave power to an object according to a power profile.
  • a power profile provides a prescribed amount of power to be applied to the object as a function of time.
  • the power profile is constructed from a plurality of segment types and types of power changes.
  • the segment types and types of power changes are selected from the list comprising: Rate, Dwell, Step, Time, GoBack, Wait, Call and End.
  • a ramp segment In order to control the rate of change of applied power, a ramp segment can be used.
  • a ramp segment provides a controlled change of setpoint from an original to a target setpoint. The duration of the ramp is determined by the rate of change specified. The segment is specified by the target setpoint and the desired ramp rate.
  • a dwell segment In order to control the power at a constant level for a specified period, a dwell segment can be used. In a dwell segment, the setpoint remains constant for a specified period at the specified target. The operating setpoint of a dwell is inherited from the previous segment.
  • a step segment For a step segment, the setpoint changes instantaneously from its current value to a new value at the beginning of a segment.
  • a step segment has a minimum duration of 1 second.
  • a time feature defines the duration of the segment.
  • the target setpoint is defined and the time taken to reach this value.
  • a dwell period is set by making the target setpoint the same value as the previous setpoint.
  • a GoBack feature is provided which allows segments to be repeated a number of times.
  • a wait feature which specifies a criterion according to which a segment cannot proceed to the next segment. Any segment can be defined as 'Wait'.
  • the imaging device comprises an infrared camera.
  • the camera allows capturing image data indicative of a temperature distribution in a product which is treated in the microwave applicator.
  • the camera then provides real-time input data which can be used by the controller to adapt the power at which the microwaves are applied to the product based on the captured image data.
  • the imaging device is sensitive to electromagnetic radiation, preferably sensitive to UV, visible, and/or IR light.
  • the imaging device is a spectral imaging device.
  • a suitable device is a hyperspectral camera.
  • IR infrared
  • multiple cameras sensitive to different parts of the electromagnetic spectrum might be used.
  • the microwave system comprises one, two or more imaging devices. Where there are two or more imaging devices, at least two may be positioned to capture image data of the product at different directions. At least 2 imaging devices may be sensitive to the same parts of the electromagnetic spectrum.
  • step b) comprises the following sub-steps: b1) providing one or more positioning blocks in the microwave applicator; and, b2) placing the product on the one or more positioning blocks.
  • the positioning blocks allow controlling the position of the product in the microwave applicator before the microwave treatment is started.
  • step g) comprises the steps: g1) determining, by the controller and based on the image data captured by the image device, an amount of excess generated microwave power; and, g2) directing, by means of a circulator, the excess generated microwave power to a dummy load.
  • the dummy load allows absorbing excess power, thereby enhancing the system's control mechanism and protecting the system against excess microwave power.
  • step g) is followed by step h) which comprises the following steps: h1) measuring an amount of incident power by means of a power meter; h2) measuring an amount of reflected power by means of a power meter; h3) determining an amount of absorbed microwave power by subtracting the amount of incident power and the amount of reflected power; h4) either using the amount of absorbed microwave power as an approximation of the amount of microwave power that was absorbed by the product; or, calculating an amount of cavity losses, and calculating the amount of microwave power that was absorbed by the product by subtracting the amount of cavity losses from the amount of absorbed microwave power.
  • the product is a liquid product
  • the method further comprises the step of stirring the product.
  • the product is moved during microwave treatment by means of a turntable.
  • a turntable is a possible alternative for a stirrer, especially for solid objects.
  • the product is subjected to ultrasound during microwave treatment.
  • the product is moved during microwave treatment by means of an ultrasound aid.
  • an ultrasound aid is a vibrating bar.
  • the vibrating bar can, for example, protrude through one of the openings in the cavity.
  • the bar comprises a non-metallic material. This helps maintaining an optimum energy distribution.
  • a vibrating table with positioning blocs is a valuable alternative to a vibrating bar.
  • a turntable, an ultrasound bar and/or a stirrer may be used together.
  • a PTFE container is preferably used.
  • step f) further comprises the step of determining a temperature distribution in the product based on the image data, and in step g), the applied microwave power to the product is further controlled based on a maximum, average, or minimum value of the temperature distribution in the product.
  • the applied microwave power is further controlled by means of a power limiter that limits the maximum applied microwave power.
  • the method employs a microwave system as described herein.
  • a microwave system for subjecting a product to a microwave treatment.
  • the system is configured for executing a method as provided herein.
  • the system comprises a microwave applicator, an imaging device, a controller, and a microwave generator.
  • the controller is operationally coupled with the microwave applicator, the imaging device, and the microwave generator.
  • the microwave generator is arranged to generate microwaves at a pre-determined power.
  • the system is arranged to subject the product to the microwaves.
  • the imaging device is arranged to capture image data indicative of a temperature distribution in the product.
  • the controller is arranged to adapt the power at which the microwaves are applied to the product based on the captured image data.
  • the microwave generator has a power between 250 W and 2000 W, or between 500 W and 1750 W, or between 750 W and 1500 W, or between 1000 W and 1250 W.
  • the system further comprises one or more wave guides, a circulator, a coupler, a power meter, a sub-tuner module, a multi-purpose module, and/or a weighing scale.
  • the system further comprises one or more of the following ancillary components: a microwave applicator door, an infrared camera, a vacuum suction line, a pressure gauge, a vacuum sensor, a pressure feed, a vacuum bleed line, a vacuum pump, an integrated water pump and chiller, and/or a product discharge and collection device.
  • ancillary components a microwave applicator door, an infrared camera, a vacuum suction line, a pressure gauge, a vacuum sensor, a pressure feed, a vacuum bleed line, a vacuum pump, an integrated water pump and chiller, and/or a product discharge and collection device.
  • the microwave applicator comprises a plurality of openings for ancillary components.
  • the microwave applicator comprises an opening that allows for operational coupling with the microwave generator.
  • the opening is sealed in an airtight manner, for example with a sheet that is transparent to microwaves, for example a plastic sheet, for example with a PTFE (polytetrafluoroethylene) sheet.
  • the system comprises a discharge and collection device as described herein.
  • the microwave system has a width between 2.0 and 3.0 m.
  • the microwave system has a height between 1.0 and 1.4 m.
  • the microwave applicator has a volume between 67 dm 3 and 77 dm 3 .
  • the magnetron has a power between 1.0 and 3.0 kW.
  • the microwave applicator is equipped with means for providing a vacuum and/or over-pressure.
  • the maximum over-pressure is limited to at most 2.0 bar.
  • the system comprises a stirrer. This is useful for homogenizing liquid objects which are treated.
  • the system comprises a turn table. This is useful for applying uniform power to a solid object.
  • the system comprises a power limiter for limiting the power applied to the object according to a pre-determined power profile.
  • the microwave applicator is a multi-mode applicator.
  • the microwave applicator is configured to treat an amount of material in the range of at least 10.0 gram to at most 3.0 kg.
  • the microwave applicator is made of stainless steel, e.g. AlSl304.
  • the microwave applicator is mounted on a steel base plate with wheels.
  • the cavity has a door which is equipped with one or more of, preferably all of, the following types of sealing: Copper alloy spring contactor for the protection for MW radiation; Teflon seal for the protection against irradiated heat; and/or Rubber seal for the air-tightness of the cavity.
  • the cavity comprises an opening for temperature monitoring by means of an imaging device, e.g. an infrared or hyperspectral camera.
  • an imaging device e.g. an infrared or hyperspectral camera.
  • this opening also allows access for a vacuum suction line.
  • the microwave applicator comprises: an opening for discharge of dried product; one or more openings for various purposes. Preferably, these openings can be sealed when not in use, e.g. by means of a steel plate; one or more pressure sensors, one or more vacuum sensors, and an opening for the pressure and vacuum sensors; a pressure feed and an opening for a pressure feed; and/or a waveguide and vacuum seal plate.
  • the vacuum seal plate is preferably made of a plastic which is transparent to microwaves such as polytetrafluoroethylene (PTFE).
  • the present systems employ a camera for temperature control.
  • the imaging device is a spectral imaging device.
  • the imaging device is positioned outside the cavity.
  • the connection between imaging device and cavity is preferably sealed with a "window" in order to enhance the vacuum in the chamber.
  • the window is made from a material which is transparent to the wavelengths employed by the imaging device for imaging. For example, when an infrared camera is used, the window is transparent to infrared light. If there is a "window" between the camera and the object of measurement, the transmissivity of the window is preferably known.
  • the microwave system is equipped with an emergency stop button, which is positioned, for example, in the door panel of an associated electrical cabinet.
  • the entire system including any installed vacuum pump, water pump, and/or chiller, is configured to shut down when the emergency stop button is pressed.
  • the door frame of the cavity is equipped with one or more, for example two, pressure sensors for detecting whether or not the door is closed.
  • the magnetron cannot be started if the cavity door is open, or if at least one of the sensors has failed.
  • the system comprises a vacuum suction line.
  • the vacuum suction line allows drying under vacuum.
  • the microwave system comprises a vacuum pump which is preferably connected to its dedicated power point.
  • a vacuum pump which is preferably connected to its dedicated power point.
  • it is operated manually by turning the power on or off.
  • the vacuum suction line is disposed with an intermediate reservoir. This extends the life-time of the vacuum pump when corrosive fumes are released during microwave treatment of the object in the microwave applicator.
  • a vacuum bleed valve is provided in fluid connection with the cavity, preferably via an opening. When creating the vacuum, this valve is closed and when removing the vacuum, the bleed valve is opened.
  • the valve can be also used for controlling (lowering) the vacuum level.
  • the vacuum level in the cavity is measured by a pressure meter on the top of the cavity.
  • a valve beneath the vacuum sensor is opened when the vacuum level is measured, and the valve is closed when no vacuum level is being measured. This reduces the chance of vacuum leaks.
  • the cavity is equipped with a pressure gauge and a vacuum sensor. Preferably, they are operationally connected to the cavity via an opening. Preferably, when vacuum is applied, a valve below the over-pressure meter closes and vice versa.
  • the cavity is further equipped with a pressure feed line and a vacuum bleed line.
  • the pressure feed line and the vacuum bleed line are operationally connected with a bleed valve which serves to control the vacuum level and for removing the vacuum (i.e. to bring the cavity to atmospheric pressure).
  • the cavity is subjected to a pressure of no more than 2 bar.
  • the system operates at 2.45 GHz.
  • the system comprises a turn table for moving the object during microwave treatment.
  • the system further comprises one or more additional sensors selected from the list comprising weight sensors, volatile organic compound sensors, pressure sensors, and temperature sensors.
  • the imaging device comprises an infrared camera.
  • the imaging device comprises a spectral imaging device.
  • the system further comprises one or more positioning blocks for supporting the product.
  • the system further comprises a circulator and a dummy load, wherein the controller is further configured to determine an amount of excess generated microwave power based on the image data captured by the image device; and wherein the circulator is configured for directing the excess generated microwave power to a dummy load.
  • the system further comprises a power meter for measuring an amount of incident power and a power meter for measuring an amount of reflected power, wherein the controller is configured to determine an amount of absorbed microwave power by subtracting the amount of incident power and the amount of reflected power, optionally wherein the controller is further configured for calculating an amount of cavity losses, and calculating the amount of microwave power that was absorbed by the product by subtracting the amount of cavity losses from the amount of absorbed microwave power.
  • the system further comprises a stirrer.
  • the stirrer comprises a glass stirring rod.
  • the system further comprises a power limiter.
  • a power limiter This improves the control of the present system. Compared to ordinary PID controllers (proportional-integral-derivative controller), the operation of the methods may be improved because of rapid microwave response times. Therefore, a power limiter can be used to limit the maximum applied power to the object. Alternatively, the power limiter may set a maximum absorbed power.
  • the power limiter is controlled according to a power profile that provides a maximum applied or absorbed power as a function of time. Accordingly, the maximum power can be adapted depending on the stage of the process.
  • the present systems and methods are especially suitable for drying porous products, wood, and clay.
  • glycerol When the system is used for assisting a chemical reaction, glycerol may be used as a reaction solvent.
  • a discharge and collection device comprises an upper valve and a lower valve for product transfer.
  • the discharge and collection device can be operationally coupled with a microwave applicator. Such a device is useful, for example, when absorption of moisture in the air by a dried product is to be avoided.
  • the product discharge and collection device comprises an upper valve and a lower valve. During the drying process both valves of the system are closed. When the drying is finished (magnetron is off, but the cavity is still under vacuum), the upper valve is opened first and, then, the lower valve. The locking mechanism of these valves requires that the handle is pulled before turning it. When the upper valve is opened, the bottom of the drying vessel opens and the product falls to the collector chute. Furthermore, the product is transferred to the collection tank by opening the lower valve. After the discharge, the collection tank is kept under vacuum by closing the lower valve. After the vacuum is removed from the cavity and the collector chute, the collector tank with the dry product under vacuum can be detached from the unit. Notice, that if the product discharge and collection device is not in use, the connection is preferably sealed with a steel plate.
  • the discharge and collection device comprises an upper valve and a lower valve for product transfer.
  • the method comprises the following steps:
  • Fig. 1 shows a microwave system (100) it comprises a microwave applicator (200), which is also called a cavity; an infrared camera (220), a controller (300), a microwave generator (400), also called magnetron; a wave guide (450), a circulator (500), another waveguide (520), a coupler (540), a power meter (550), a sub-tuner module (600), a multi-purpose module (700), a weighing scale (800), and an ultrasound aid (1000).
  • a microwave applicator 200
  • an infrared camera 220
  • a controller 300
  • a microwave generator also called magnetron
  • a wave guide 450
  • a circulator 500
  • another waveguide 520
  • a coupler 540
  • a power meter a sub-tuner module
  • 700 multi-purpose module
  • weighing scale 800
  • an ultrasound aid 1000
  • Fig. 2 shows a microwave intensity pattern in a microwave applicator (200). The microwave intensity is not constant throughout the microwave applicator (200).
  • Fig. 4 shows a various ancillary components of the microwave applicator (200).
  • the microwave applicator comprises, or is associated with, the following components: a microwave applicator door (210), an infrared camera (220), a vacuum suction line (230), a pressure gauge (240), a vacuum sensor (250), a pressure feed (260), a vacuum bleed line (270), a vacuum pump (280), an integrated water pump and chiller (285), and a product discharge and collection device (290).
  • Fig. 5 shows the inside of the microwave applicator (200), and particularly highlights a plurality of openings(201,202,203,204,205,206,207) for ancillary components.
  • One opening (207) allows operational coupling with the microwave generator (400).
  • This opening (207) is provided with a PTFE sheet (2071) which is transparent to microwaves.
  • Fig. 6 shows a product discharge and collection device (290) which employs an upper valve (291) and a lower valve (292) for product transfer.
  • the system When the system is used for processing liquid objects, a stirrer is provided for homogenizing the mixture. Additionally or alternatively, the system comprises a turn table.
  • the system comprises a power limiter for limiting the power applied to the object according to a pre-determined power profile.
  • the controller (300) is a general purpose controller which controls the various components of the microwave system (100)
  • the microwave applicator (200) is a multi-mode applicator that uses microwave energy to treat material from tens of grams to three kg at a time. It is designed for experimental use or for batch production in small scale.
  • the cavity i.e. the hollow space inside the microwave applicator 200
  • the framework are made of stainless steel (AlSl304) and are mounted on a steel base plate with wheels.
  • the microwave applicator (200) is suitable for use as a drying unit. It should be placed in a well-ventilated place, where the ambient temperature does not exceed 30°C. The microwave-proof door is closed and secured during the operation of the device.
  • any object (reservoirs, beakers, etc.) that is put in the cavity should be clean and made of material that does not couple with microwaves. Because microwaves are applied, there should not be any metal objects lying around the device.
  • the object is positioned in a desired position by means of one or more positioning blocks.
  • the microwave applicator (200) and its door (210) are certified for vacuum and over-pressure up to 2 bar and it is closed with ten bolts (M18).
  • M18 ten bolts
  • associated butterfly nuts are tightened firmly and evenly.
  • equal force should be applied with each bolt. Too high load affects the life-time of the bolts, but first of all, it may damage the "saw-toothed" copper alloy lining (spring contactor) around the cavity opening that is used for an additional protection against MW radiation. Furthermore, an uneven load may cause MW leakages.
  • the cavity door has three types of sealing:
  • the cavity (200) has seven through holes/openings (201-207) at different locations, that can be used for various purposes and set-ups.
  • the inside of the cavity (200) is shown in Figure 5 .
  • the cavity (200) comprises the following openings:
  • an opening (203,204) is used for temperature control by a camera (not shown in the figures).
  • suitable cameras are infrared cameras and hyperspectral cameras (spectral imaging devices).
  • the camera positioned outside the cavity (200).
  • the connection is preferably sealed with a "window" (in order to enhance the vacuum in the chamber) that is specially made for this purpose (special IR transparent material). If there is a "window" between the camera and the object of measurement, the transmissivity of the window is preferably known.
  • the microwave system comprises one, two or more imaging devices. Where there are two or more imaging devices, at least two may be positioned to capture image data of the product at different directions. At least 2 imaging devices may be sensitive to the same parts of the electromagnetic spectrum.
  • temperature monitoring is performed by an infrared (IR) camera.
  • IR radiation infrared
  • This non-contact method measures the radiation of heat (IR radiation) from an object.
  • a parallel method (not IR based - e.g. thermocouple) may be used, for example by means of the following procedure: the temperature of a specific material is measured both by the IR sensor and the comparative method. By decreasing or increasing the emissivity value the temperature reading of the IR sensor is adjusted to correspond the measured temperature by the comparative method.
  • the factory setting of the emissivity is 0,95.
  • the camera allows capturing image data indicative of a temperature distribution in in a product which is treated in the microwave applicator.
  • the controller (300) of the microwave system (100) then adapts the power at which the microwaves are applied to the product based on the captured image data.
  • the system comprises a circulator and a dummy load.
  • a controller in the system determines an amount of excess generated microwave power based on the image data captured by the image device. Then, the circulator directs excess generated microwave to the dummy load, where it is absorbed.
  • the system further comprises a power meter for measuring an amount of incident power and a power meter for measuring an amount of reflected power.
  • the system comprises a controller which is configured to determine an amount of absorbed microwave power by subtracting the amount of incident power and the amount of reflected power. The can also take into account cavity losses.
  • the controller is further configured for calculating an amount of cavity losses, and calculating the amount of microwave power that was absorbed by the product by subtracting the amount of cavity losses from the amount of absorbed microwave power.
  • the microwave system (100) is equipped with an emergency stop button in the door panel of an associated electrical cabinet. After pressing it, the whole microwave system (100) shuts down, including the vacuum pump (280), and the integrated water pump and chiller (285). The alarm indicator light will be on until the emergency stop button is released and the system is reset by pushing a reset button. The emergency stop button is released by pulling the knob of the button back.
  • the door frame of the cavity (200) has two pressure sensors for detecting if the door is closed or not.
  • the magnetron (400) is controlled by these sensors. In other words, the magnetron (400) cannot be started if the cavity door is open (one or both sensors fail).
  • cooling water is useful for two distinct purposes: 1) Feeding water to the isolator that prevents the mis-matched (reflected) microwaves to bounce back to the magnetron; and 2) cooling the magnetron.
  • the water circuit significantly improves the operation of the microwave oven and the life expectancy of the electronics inside.
  • the microwave (MW) unit is preferably not operated without a supply of cooling water at the correct temperature. This can be enforced by requiring, for example, that the magnetron will not start if the water flow is too low or if the cooling water is too hot.
  • the water is circulated by a pump that is integrated with a chiller.
  • the water pump and chiller are comprised in an integrated water pump and chiller (285).
  • the total water volume of the system is 10 liters.
  • the level of the water is preferably between the maximum and minimum lines in the level meter of the cooling unit.
  • the water used is preferably solids-free and does not contain any organic contaminants, such as, oils. Distilled water or potable water are suitable for this purpose.
  • the microwave system (100) is further equipped with pressure regulating devices including a vacuum suction line (230), pressure gauge (240), vacuum sensor (250), pressure feed (260), vacuum bleed line (270), and a vacuum pump (280).
  • pressure regulating devices including a vacuum suction line (230), pressure gauge (240), vacuum sensor (250), pressure feed (260), vacuum bleed line (270), and a vacuum pump (280).
  • the vacuum suction line (230) allows drying under vacuum.
  • the purpose of drying under vacuum is to lower the boiling point of the liquid (water). When the evaporation takes place at lower temperature, the product heats less and, therefore, the drying process is more gentle to the product. In addition, less energy is required for heating.
  • the vacuum pump (280) is connected to its dedicated power point and operated manually by turning the power on or off.
  • a vacuum bleed valve is provided in fluid connection with the cavity (200) via an opening (206). When creating the vacuum, this valve is closed and when removing the vacuum, the bleed valve is opened. Optionally, the valve can be also used for controlling (lowering) the vacuum level.
  • the vacuum level in the cavity is measured by a pressure meter on the top of the cavity (opening 205).
  • a valve beneath the vacuum sensor is opened.
  • the cavity (200) is equipped with a pressure gauge (240) and a vacuum sensor (250). They are operationally connected to the cavity via an opening (205). When vacuum is applied, a valve below the over-pressure meter closes and vice versa.
  • the cavity (200) is further equipped with a pressure feed line (260) and a vacuum bleed line (270).
  • the pressure feed line (260) and the vacuum bleed line (270) are operationally connected with a bleed valve which serves to control the vacuum level and for removing the vacuum (i.e. to bring the cavity (200) to atmospheric pressure).
  • the cavity (200) is subjected to a pressure of no more than 2 bar.
  • the cavity (200) is further equipped with a product discharge and collection device (290) for collecting dried product.
  • This device (290) is particularly useful for preventing any absorption of the moisture in the air by treated products.
  • the product discharge and collection device (290) the dry product is transferred from the cavity to the collection tank under vacuum.
  • the discharge and the collection device (290) of the dried product is shown in Figure 6 .
  • the product discharge and collection device (290) comprises an upper valve (291) and a lower valve (292). During the drying process both valves of the system are closed. When the drying is finished (magnetron is off, but the cavity is still under vacuum), the upper valve (291) is opened first and, then, the lower valve (292). The locking mechanism of these valves requires that the handle is pulled before turning it.
  • the upper valve (291) When the upper valve (291) is opened, the bottom of the drying vessel opens and the product falls to the collector chute. Furthermore, the product is transferred to the collection tank by opening the lower valve (292). After the discharge, the collection tank is kept under vacuum by closing the lower valve (292).
  • the collector tank with the dry product under vacuum can be detached from the unit. Notice, that if the product discharge and collection device (290) is not in use, the connection is preferably sealed with a steel plate.
  • the microwave applicator (200) is equipped with an ultrasound aid (1000) that can be used for applying to a product under microwave treatment.
  • Microwave heating scaling-up constitutes a growing demand for industry due to the great success obtained in chemical reactions at laboratory scale and so, a great opportunity to enhance industrial processes.
  • the microwave penetration for most of solvents is around a few centimeters for the most commonly used microwave frequency, 2.45 GHz.
  • controlling the stirring rate in order to maintain a homogeneous solution and avoid thermal gradients is preferably taken into account.
  • most of the reactions accomplished under microwave irradiation are performed at high temperatures in sealed vessels.
  • Various approaches and processing techniques can be used for scaling-up a wide range of reactions.
  • the used set up is a multipurpose test device for various microwave applications.
  • the design has entries on the sides of the cavity allowing multiple connections for sensors and entrances/exits for gas or products.
  • the opening on the right side was used to measure the temperature of the sample by means of an infrared (IR) camera, while the opening on top was used to insert the glass stirring rod. Different matter properties were studied.
  • the emissivity of matter can be defined as the effectiveness in emitting energy as thermal irradiation and varies from 0 to 1.
  • matter transmissivity refers to the proportion of the radiation that hits a body and ends up being transmitted through it without being absorbed or reflected. Both were measured in our reaction solvent, glycerol.
  • the emissivity of glycerol was calculated by comparing the solution temperature with a thermometer and with a microwave IR camera, and the factor was 0.95. While the emissivity value is intrinsic and only depends on the solution nature, the transmissivity value depends also on the vessel form and material. In our case the value of transmissivity results in 0.48.
  • the IR camera is always positioned in the same point in order to maintain constant parameter values. Once those parameters were set up, different experiments were performed.
  • process intensification means a great promise for sustainable synthesis.
  • Effects of microwave and ultrasound irradiation have been studied for the synthesis of aniline by the chemicoselective reduction of nitrobenzene with copper nanoparticles in glycerol as green reducing agent and solvent.
  • Metal catalyzed reactions are known to be one of the favorite fields of ultrasound assisted reactions.
  • previous ultrasound treatment shows to have a beneficial effect since it provides a homogeneous distribution of metal particles in the solution media and so, a higher catalytic surface.
  • the reduction reaction was accomplished using different microwave devices, mono- and multimode. In all cases, the selection of a constant power method showed to have a positive effect in the reaction outcome. Generation of active species in the reaction media and superheating when working at high microwave power could accelerate the reaction.
  • the system comprises a microwave applicator (200), an imaging device (220), a controller (300), and a microwave generator (400).
  • image data indicative of a temperature distribution of the product are captured by means of an infrared camera. Based on these image data, the applied microwave power to the product is controlled.
  • an amount of excess generated microwave power is determined by the controller based on the image data captured by the image device.
  • the excess power is then directed to a dummy load (600) by means of a circulator (500).
  • the power delivered to the product to be processed is controlled by measuring an amount of incident power and an amount of reflected power by means of one or more power meters. Then, an amount of absorbed microwave power is determined by subtracting the amount of incident power and the amount of reflected power. The amount of absorbed microwave power is either used as an approximation of the amount of microwave power that was absorbed by the product, or an amount of cavity losses is calculated and the amount of microwave power that was absorbed by the product is then calculated by subtracting the amount of cavity losses from the amount of absorbed microwave power.
  • the applied microwave power to the product is further controlled by 1) determining a temperature distribution in the product based on the image data, and 2) a maximum, average, or minimum value of the temperature distribution in the product.
  • the applied microwave power is further controlled by means of a power limiter that limits the maximum applied microwave power.
  • the following procedure can be followed: a) ascertain the weight of the collector tank with its vacuum seal (tare); b) ascertain the initial moisture and weight of the product (measured by, e.g., IR scale); c) calculate the theoretical weight loss based on the initial moisture content and the desired end moisture content; and d) check the dryness of the material by weighing.
  • the infrared camera is used for temperature control.
  • the microwave system (100) allows to apply a power profile to a sample.
  • the present example illustrates how a power profile can be constructed from a series of segments.
  • the segments describe the evolution of the power during a pre-determined time period.
  • Various segment types are illustrated in Figure 7 .
  • a ramp segment ( Fig. 7 panel a)) can be used.
  • a Ramp segment provides a controlled change of setpoint from an original to a target setpoint. The duration of the ramp is determined by the rate of change specified. The segment is specified by the target setpoint and the desired ramp rate. The ramp rate parameter is presented in engineering units (°C, °F) per real time units (Seconds, Minutes or Hours).
  • a dwell segment ( Fig. 7 panel b)) can be used. In a dwell segment ( Fig. 7 panel b), the setpoint (i.e. the applied power) remains constant for a specified period at the specified target. The operating setpoint of a dwell is inherited from the previous segment
  • the setpoint changes instantaneously from its current value to a new value at the beginning of a segment.
  • a step segment has a minimum duration of 1 second.
  • a time feature defines the duration of a segment.
  • the target setpoint is defined and the time taken to reach this value.
  • a dwell period is set by making the target setpoint the same value as the previous setpoint.
  • a GoBack feature is provided which allows segments to be repeated a number of times.
  • a wait feature which specifies a criterion according to which a segment cannot proceed to the next segment. Any segment can be defined as 'Wait'.

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  • Physics & Mathematics (AREA)
  • Electromagnetism (AREA)
  • Drying Of Solid Materials (AREA)
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