WO2013070095A1 - Appareil à micro-ondes et procédés associés - Google Patents

Appareil à micro-ondes et procédés associés Download PDF

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Publication number
WO2013070095A1
WO2013070095A1 PCT/NZ2012/000210 NZ2012000210W WO2013070095A1 WO 2013070095 A1 WO2013070095 A1 WO 2013070095A1 NZ 2012000210 W NZ2012000210 W NZ 2012000210W WO 2013070095 A1 WO2013070095 A1 WO 2013070095A1
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WO
WIPO (PCT)
Prior art keywords
cavity
microwave
resonant
substance
feed
Prior art date
Application number
PCT/NZ2012/000210
Other languages
English (en)
Other versions
WO2013070095A9 (fr
Inventor
Murray Friar
Richard John Futter
Original Assignee
Cquest Technology Limited
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
Priority claimed from AU2012202004A external-priority patent/AU2012202004A1/en
Application filed by Cquest Technology Limited filed Critical Cquest Technology Limited
Publication of WO2013070095A1 publication Critical patent/WO2013070095A1/fr
Publication of WO2013070095A9 publication Critical patent/WO2013070095A9/fr

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Classifications

    • 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
    • H05B6/701—Feed lines using microwave applicators
    • 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
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J19/12—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electromagnetic waves
    • B01J19/122—Incoherent waves
    • B01J19/126—Microwaves
    • 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
    • H05B6/707—Feed lines using waveguides
    • 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
    • H05B6/806—Apparatus for specific applications for laboratory use
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/0873—Materials to be treated
    • B01J2219/0892—Materials to be treated involving catalytically active material
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/12—Processes employing electromagnetic waves
    • B01J2219/1203—Incoherent waves
    • B01J2219/1206—Microwaves
    • B01J2219/1275—Controlling the microwave irradiation variables
    • B01J2219/1281—Frequency

Definitions

  • the invention relates to an energy transfer apparatus including a microwave cavity for transfer of energy to substances fed through the cavity.
  • the invention also relates to associated methods of processing substances.
  • the invention relates to a method of pyrolysis of organic substances, such as polychlorinated organic substances, as a continuous process and an apparatus adapted for use in the continuous processing of the organic substances by the method of pyrolysis.
  • Plastic makes up a considerable portion of the organic substances present in municipal waste. With reducing volumes of solid municipal waste being permitted to be disposed of as landfill, many municipalities are resorting to incineration as a means of disposal. Plastic present in municipal waste includes chlorinated types such as polyvinyl chloride (PVC). This form of chlorinated organic substance is the third most common type of plastic produced on a worldwide basis.
  • PVC polyvinyl chloride
  • Incineration of solid municipal waste comprising chlorinated organic substances may result in the release of by-products including polyaromatic hydrocarbons (PAH), polychlorinated dibenzyl furans (PCBF) and polychlorinated dibenzyl dioxins (PCBD).
  • PAH polyaromatic hydrocarbons
  • PCBF polychlorinated dibenzyl furans
  • PCBD polychlorinated dibenzyl dioxins
  • microwave cavities for energy transfer in industrial settings, including the processing of municipal waste.
  • the use of microwave cavities in such settings has not been widely accepted due to a number of disadvantages.
  • Existing systems suffer from poor performance, with low efficiency of energy transfer.
  • the publication cites the use of the microwave apparatus in the processing by pyrolysis of organic substances, but does not address the problem of the hazardous by-products that may be released during the pyrolysis of chlorinated organic substance. Further, the efficiency achieved by the apparatus described leaves further room for improvement. It is an object of the present invention to provide an improved microwave cavity energy transfer apparatus and/or improved reaction method.
  • the invention provides a method of processing an organic substance comprising the step of feeding a blend of the organic substance and a catalyst along a path substantially parallel to a longitudinal node axis of a resonant mode pattern of microwave radiation in an elongate resonant cavity where the microwave energy supplied to the blend in the resonant cavity is sufficient to achieve pyrolysis of the organic substance.
  • the microwave energy supplied to the blend in the resonant cavity is sufficient to achieve greater than 95% by weight of pyrolysis of the organic substance.
  • the microwave energy supplied to the blend in the resonant cavity is sufficient to achieve greater than 99% by weight of pyrolysis of the organic substance.
  • the organic substance is selected from the group consisting of: halogenated organic substances, municipal waste, treated timber and vulcanised rubber. More preferably, the organic substance is selected from the group consisting of: organic substances anticipated to contain chlorinated organic substances. Most preferably, the organic substance is selected from the group consisting of: organic substances anticipated to contain chlorinated plastics.
  • the method is effective to mitigate the risk of the release to the environment of volatilised hazardous by-products arising from the thermal decomposition of these organic substances.
  • the catalyst is capable of binding halogen as halide.
  • the catalyst is capable of binding chlorine as chloride. More preferably, the catalyst is capable of binding chlorine as inorganic chloride. Most preferably, the catalyst comprises iron (II, III) oxide.
  • the catalyst is capable of binding sulphur as sulphide.
  • the catalyst is capable of binding hydrogen sulphide. More preferably, the catalyst comprises carbon.
  • the catalyst is selected from the group consisting of: carbon, iron (II, III) oxide, nickel, titanium dioxide, titanomagnetite and mixtures thereof. More preferably, the catalyst is selected from the group consisting of: iron (II, III) oxide and mixtures of iron (II, III) oxide with one or more of carbon, nickel, titanium dioxide. Most preferably, the catalyst comprises a mixture of iron (II, III) oxide and carbon.
  • the method is performed in a non-oxidizing atmosphere. More preferably, the method is performed in a reducing atmosphere. Most preferably, the method is performed in an atmosphere comprising hydrogen and nitrogen.
  • the method is performed at a pressure above atmospheric pressure.
  • the method of processing the organic substance is a continuous method of processing the organic substance.
  • the resonant mode pattern of microwave radiation is established in a single mode resonant microwave cavity.
  • the path is substantially parallel to and offset from the longitudinal node axis of the resonant mode pattern of microwave radiation.
  • the invention provides an apparatus comprising a microwave source, an elongated resonant cavity connected to the microwave source via a waveguide, a conduit passing along the length of the resonant cavity from an inlet to an outlet and a source of substance configured to supply the substance to the inlet of the conduit at a feed rate, where the conduit is arranged substantially parallel to and offset from a longitudinal node axis of a natural resonant mode pattern of the resonant microwave cavity.
  • the resonant cavity is connected to the microwave source by a waveguide and the feed conduit is offset from the longitudinal node axis in a direction directly away from the waveguide.
  • the apparatus has a natural resonant frequency of any one of 2450 MHz, 915 MHz or 850 MHz.
  • the cavity is substantially formed from a conductive material.
  • the conduit and/or the substance perturb the resonant mode of the cavity such that the offset conduit is aligned with two or more nodes of the perturbed resonant mode.
  • the conduit is formed from a material that is substantially transparent to microwaves at an operating temperature of the apparatus.
  • the apparatus is configured for adjustment of the relative positions of the conduit and cavity such that the offset is adjustable.
  • the offset is adjustable in real time.
  • the resonant cavity is defined by one or more side walls and two cavity ends, each cavity end comprising an end wall having an aperture therein and a sleeve extending from the end wall to the outside of the cavity and having a hollow bore communicating with the aperture, such that the end wall and the sleeve together present a substantially reflective surface to microwave energy in the cavity.
  • the cavity is connected to the microwave source by a waveguide and the apparatus comprises a microwave detection arrangement configured to monitor microwave energy travelling in the waveguide away from the cavity, an adjustable tuner positioned on the waveguide and a controller configured to control adjustment of the tuner in order to minimize the microwave energy travelling in the waveguide away from the cavity.
  • the microwave detection arrangement comprises one or more directional couplers.
  • the microwave detection arrangement is also configured to monitor microwave energy travelling in the waveguide towards the cavity.
  • the adjustable tuner is a three stub tuner.
  • the adjustable tuner is capable of adjusting the waveguide impedance to match the cavity's impedance over an operational range.
  • the apparatus comprises one or more sensors configured to measure one or more properties of the substance after it has passed through the cavity and a controller configured to control one or more operating parameters of the apparatus in response to those measurements.
  • the one or more sensors comprise a temperature sensor.
  • the temperature sensor is an optical pyrometer configured to measure a temperature of the feed conduit and therefore of the substance.
  • the one or more sensors comprise a chemical sensor configured to detect one or more chemicals in the substance.
  • the operating parameters comprise one or more of a feed rate of the substance through the feed conduit; microwave source power; and/or the offset.
  • the apparatus comprises a reaction suppressant source connected to the feed conduit and configured to introduce a reaction suppressant into the feed conduit.
  • the apparatus comprises one or more sources of further substances connected to the conduit and configured to introduce the further substances into the conduit.
  • the further substances may include one or more reagents and/or catalysts.
  • the invention provides an apparatus comprising a microwave source, a resonant cavity connected to the microwave source, a feed conduit passing through the resonant cavity from an inlet to an outlet, a source of substance configured to supply substance to the inlet of the conduit at a feed rate, one or more sensors configured to sense one or more parameters of material after it has passed through the cavity, a controller configured to receive information from the one or more sensors and to adjust in real time one or more of the feed rate, power supplied by the microwave source and/or a position of the feed conduit within the microwave cavity, in order to achieve a desired transfer of power from a resonant microwave field in the resonant cavity to substance passing through the conduit.
  • the invention provides a continuous microwave heating or reaction apparatus comprising a microwave source, a resonant cavity, a waveguide connecting the resonant cavity to the microwave source, a conduit passing through the resonant cavity from an inlet to an outlet, a source of substance configured to supply substance to the inlet of the conduit at a feed rate, one or more sensors configured to sense reflected microwave radiation within the waveguide, a controller configured to receive information from the one or more sensors and to perform one or more of the following: adjust in real time one or more adjustable tuners to improve the impedance matching between the waveguide and the resonant cavity, thereby reducing the reflected microwave radiation; interpret the information to determine reaction parameters within the feed tube; and adjust in real time one or more of: the feed rate; power supplied by the microwave source; and a position of the conduit within the microwave cavity.
  • the invention provides a staged reaction method in a microwave heating or reaction apparatus, the apparatus including a resonant microwave cavity; the method including: establishing a resonant microwave mode in the resonant microwave cavity, the resonant microwave mode including at least a first node and a second node, each node defining a region of high energy transmission from the resonant microwave mode to a feed substance passing through the cavity; passing the feed substance through the first node, microwave energy transmitted to the feed substance at the first node causing a first reaction stage to occur, the first reaction stage including one or more first chemical reactions within the feed substance, creating a partially reacted feed substance; and passing the partially reacted feed substance through the second node, microwave energy transmitted to the partially reacted feed substance at the second node causing a second reaction stage to occur, the second reaction stage including one or more second chemical reactions within the partially reacted feed substance.
  • the apparatus includes a microwave source and establishing a resonant microwave mode in the resonant microwave cavity includes introducing microwave energy from the microwave source into the resonant microwave cavity.
  • At least one of the second chemical reactions has a higher activation energy than any of the first chemical reactions, and the second node provides greater energy transfer to the feed substance than the first node.
  • the invention provides a method of the first or fifth aspect of the invention performed in an apparatus of the second, third or fourth aspect of the invention.
  • Chlorinated means chlorine bound by covalent bonds.
  • Consisting of means excluding any element, ingredient or step not specified except for impurities and other incidentals.
  • Halogenated means halogen bound by covalent bonds.
  • Node means a region of high energy transfer from the resonant microwave mode to a feed substance located at the node.
  • “Pyrolysis” means the thermal decomposition of a substance by cleavage of covalent bonds to provide volatile components and a carbonaceous residue.
  • “Resonant cavity” means a cavity in which a resonant mode pattern of microwave radiation is established.
  • concentrations or ratios of substances are specified the concentrations or ratios specified are the initial concentrations or ratios of the substances. Unless otherwise specified, where concentrations or ratios of substances are specified as percentages the percentages are calculated on a 'by weight' basis.
  • 1 .7 encompasses the range 1 .650 recurring to 7.499 recurring.
  • FIG. 1 A perspective view of an energy transfer apparatus according to one embodiment.
  • Figure 2. A schematic diagram of an energy transfer system according to one embodiment.
  • FIG. 3 A microwave cavity with a representation of a natural resonant mode.
  • Figure 3A A cross-section through the cavity of Figure 3.
  • Figure 4 A microwave cavity with a representation of a perturbed resonant mode.
  • Figure 4A A cross-section through the cavity of Figure 4.
  • FIG. 1 A microwave cavity with a representation of a further resonant mode.
  • Figure 5A A cross-section through the cavity of Figure 5.
  • Figure 6 A computer model of the resonant mode in one embodiment.
  • the invention resides at least in part in the use of a resonant mode pattern of microwave radiation (i.e. radiation at 300 MHz to 300 GHz) established in a single mode or resonant cavity.
  • the cavity usually consists of a closed volume constructed of electrically conductive material (usually a metal), which presents a reflective surface to microwaves within the cavity.
  • the microwave energy establishes a resonant mode pattern or "resonant mode" within the cavity.
  • the cavity will have a number of possible resonant frequencies and resonant modes.
  • the resonant frequencies and modes will depend primarily on the dimensions of the cavity, but also on the material forming the walls of the cavity. The physics of such cavities, when operating under ideal conditions, is well understood and need not be described in detail in this specification.
  • microwave cavities in the processing of substances has a number of advantages over the use of alternative means of delivering thermal energy by convection or conduction.
  • energy is provided throughout the body of the substance exposed to the microwaves. More even heating of the substance results, rather than heating only at the surface.
  • Single mode cavities are to be contrasted with multi-mode cavities, such as those used in domestic microwave ovens.
  • a single mode cavity is a resonant cavity designed to create a resonant mode pattern of the microwave radiation.
  • a multi-mode design actively discourages long term standing waves. The radiation waves are randomly and chaotically reflected around the chamber. Specifically, there is no "resonant mode".
  • the present invention is concerned only with the use of single mode cavities.
  • a substance is processed by being fed along a path substantially parallel to the longitudinal node axis of a resonant mode pattern of microwave radiation.
  • the invention permits the continuous processing of the substance. As the substance is fed along the path it is exposed to a varying intensity of microwave radiation.
  • the method of the present invention is to be distinguished from that disclosed in the publication of Holzschuh et a/ (2007).
  • the publication of Holzschuh et a/ (2007) discloses a microwave reactor in which a fluid is conducted transversely to the direction of propagation of an electromagnetic wave in a waveguide.
  • the microwave reactor comprises both an activated chamber and a reaction chamber separated by a metal grid.
  • Robinson et al (2010) the fundamental mechanisms of microwave pyrolysis are poorly understood.
  • the varying intensity of microwave radiation provided by the substance being fed along a path substantially parallel to the longitudinal axis of the resonant mode pattern of microwave radiation results in improved catalytic outcomes, such as the magnetite catalysed dechlorination of a polychlorinated organic substance. It has been found that the efficiency with which these catalytic outcomes is obtained is further improved by the path being offset from the longitudinal node axis of the natural resonant mode pattern of microwave radiation established in the microwave cavity.
  • the publication of Lewis et al (2000) discloses an elongated chamber that is tuneable by mechanical adjustment of the cross-sectional area so as to control and maintain a microwave field uniformity and resonant mode during the processing of substances.
  • the configuration of the path being offset from the longitudinal node axis of the natural resonant mode pattern of microwave radiation appears to be optimal, e.g. for the magnetite catalysed dechlorination of polychlorinated organic substances.
  • the energy transfer provided by the configuration of the apparatus and its operation in accordance with the described method is believed to promote the cleavage of halogen-carbon, e.g.
  • the energised catalyst both promotes dechlorination and reacts with the released chlorine radicals.
  • the catalyst may also promote hydrogenation of the intermediate organic species. Such hydrogenation would reduce the likelihood of chlorinated aromatic ring stabilised by-products being formed and released as volatiles.
  • a catalyst capable of promoting these postulated reaction steps is magnetite (iron (II, III) oxide or "iron sand”), which may be amended with titanium dioxide.
  • magnetite iron (II, III) oxide or "iron sand”
  • the term "catalyst” will be understood to refer to a substance, typically an inorganic substance, which both promotes and participates in the reaction pathway that results in the pyrolysis of the organic substance.
  • the mixture of the organic substance with the catalyst is an intimate mixture (or "blend") of the organic substance and catalyst. It is anticipated that the pyrolysis via the postulated reaction steps may be further optimised by the inclusion of other components. Examples of such components include nickel, tin and/or chromium.
  • the catalyst may be a mixture including magnetite and zinc chloride.
  • the catalyst may be formed by grinding together 90% by weight of nano particulate magnetite powder with 10% by weight zinc chloride.
  • the catalyst may be formed by calcining a mixture of 70% by weight nanoparticle magnetite with 30% by weight activated carbon. A mixture of 95% by weight of the calcined material with 5% by weight zinc chloride may then be ground together to produce the catalyst.
  • the blend of organic substance and catalyst includes at least 10% by weight of magnetite. In other embodiments the blend includes around 50% by weight of magnetite.
  • the catalyst includes at least one component that effectively absorbs microwave radiation.
  • Magnetite, titanomagnetite and carbon are good absorbers of microwave radiation.
  • FIG. 1 shows an energy transfer apparatus 1 according to one embodiment.
  • the apparatus includes a microwave cavity 2 in the form of a cylindrical body 3 with perpendicular end walls 4. This type of cavity is sometimes called a right-cylindrical cavity. In some embodiments other cavity shapes, such as rectangular cross-section cavities, may be used.
  • a waveguide 6 is connected to the cavity 2 and a flange 7 allows connection of a microwave source (not shown in Figure 1 ).
  • a microwave source such as a magnetron or klystron.
  • a readily available magnetron such as used in a domestic microwave oven, may be used.
  • the source may provide microwave radiation at 2450 MHz with power outputs up to 36 kW. In another embodiment the source may provide microwave radiation at 915 MHz with power outputs up to 100 kW.
  • the waveguide 6 will have dimensions suitable to the frequency of microwave radiation to be transmitted, as is well understood in the art.
  • the source may be connected directly to the waveguide, or may be connected to the waveguide via a further transmission line of any suitable kind.
  • An isolator may be provided to protect the source from any microwave radiation that be be reflected back towards the source.
  • 2450 MHz microwave radiation may be transferred from the source to the waveguide using a microwave coaxial cable.
  • a sleeve 9 extends from each end wall 4 of the cavity 2, with each end wall having an aperture therein that meets with the hollow bore of the sleeve 9.
  • Each sleeve 9 may be formed in a single piece with the corresponding end wall 4, forming a generally top-hat shaped element.
  • the cylindrical body 3, end walls 4 and sleeves 9 together form the resonant cavity.
  • conductive coatings may be used, and these may be applied to non-conductive substrates (e.g. glass).
  • Metal coatings or plating may be used, or non-metallic conductive coatings such as nanoparticulate conductive carbon coatings (e.g. conductive nanotube coatings) may be used in some applications.
  • the material chosen will vary with the resonant frequency, due to the change in skin depth with frequency (the skin depth is smaller at higher frequencies resulting in a higher effective resistance). At high frequencies more conductive materials must therefore be used.
  • the cavity may be formed of copper (preferably high purity copper, such as 99.9% pure copper), or from a less conductive surface (e.g. brass or bronze) plated or coated with highly conductive silver or gold. Gold plating has the advantage that it is long-lived and does not tarnish.
  • a resonant frequency of 915MHz aluminium may be sufficiently conductive.
  • the conductive metal material forms a reflective surface that confines the microwave energy to the interior of the cavity.
  • the end walls 4 and sleeves 9 together form an efficient reflective unit at each end of the cavity, while defining a hollow bore that passes into the cavity.
  • the Applicant's sleeves provide an aperture through the cavity wall, but prevent significant escape or leakage of microwave energy through that aperture.
  • the sleeve 9 essentially forms a cylindrical waveguide, but the dimensions of the sleeve 9 are such that the resonant frequency of the cavity is less than the cutoff frequency of the sleeve waveguide (taking into account the presence of the feed tube which tends to increase the effective diameter of the waveguide). This means that the microwave energy does not propagate through the sleeves.
  • the cavity and sleeve arrangement may be supported by brackets 1 1 mounted to a support structure 12. However, any suitable structural arrangement may be used.
  • the waveguide 6 must also be formed from a conductive material and is preferably a metal tube type waveguide optimised for the transmission of microwave energy of the desired frequency. In the embodiment shown a rectangular waveguide is used. The physics of such waveguides is well understood and need not be discussed in detail in this specification.
  • the energy transfer apparatus 1 also includes a feed arrangement configured to continuously feed matter through the cavity.
  • the feed arrangement includes a feed tube 14, which passes through the bores in the two sleeves 9, through the apertures in the end walls 4 and through the cavity 2.
  • the feed tube 14 may be mounted by supports 15 to brackets 16 attached to the support structure 12.
  • the brackets 16 also include a connection arrangement 1 7 for connection of external flow conduits (not shown) to the feed tube 14.
  • the feed tube is preferably formed of a material that is substantially transparent to microwaves, chemically resistant to the material that will be flowing through it (reagents, catalysts etc as well as reaction products) and capable of withstanding the pressures, temperatures and temperature changes experienced in this type of apparatus (in one embodiment the temperature can change from room temperature to 1200 degrees Celsius in a matter of seconds).
  • the material required will therefore vary with the application. Further, the material's microwave transparency characteristics may also be frequency-dependent.
  • silica may be a suitable material, although silica is not useful at 2450 MHz and higher temperatures (e.g. 800 degrees Celsius) because its transparency to microwaves at this frequency decreases with temperature.
  • alumina silicate ceramics are suitable, such as those sold under the "Pythagoras" brand by Haldenwanger, part of the Morgan Crucible Company PLC.
  • alumina e.g fused alumina
  • this listing of materials is subject to the chemical resistance of the feed tube material to whatever material is flowing through the apparatus. These materials may not be suitable for some applications.
  • the feed tube may have an outside diameter of around 31 .8mm and an internal diameter of 25.4mm. In another embodiment operating at 91 5 MHz, the feed tube may have an outside diameter of around 76.2mm and an internal diameter of 69mm.
  • the cavity dimensions will depend on the desired resonant frequency and the nature of the material to be treated. For a particular material the permeability and permittivity may be estimated, and the cavity radius chosen to match the resonant frequency to the frequency of the available source. For example, if a 2450MHz magnetron is used as the source, it is desirable to have a cavity with a resonant frequency of approximately 2450MHz in the desired mode. The resonant frequency of the cavity is not dependent on the source frequency, but matching between the two is desirable.
  • the cavity has a diameter of around 76 mm, with a cavity length around 97mm.
  • the sleeves 9 may extend around 190mm from the cavity end walls and have diameters around 40.5mm.
  • the cavity has a diameter of around 203 mm, with a cavity length around 268mm.
  • the sleeves 9 may extend around 350mm from the cavity end walls and have diameters around 80mm.
  • other dimensions may be suitable and the invention is not limited in this respect.
  • the apparatus is configured to operate as a single mode cavity.
  • a resonant mode is established in the cavity, with one or more nodes where the electric field component of the microwave pattern is at a maximum. These nodes are regions of high energy transfer from the microwave pattern to the feed material. In preferred embodiments the nodes lie along one or more node axes parallel to the length of the cavity.
  • the cavity may be designed to support any desired mode.
  • Lower modes such as TE1 1 1 or TM010 may be more easily maintained.
  • the feed material may interact more strongly with the magnetic field, and an appropriate mode may be chosen to maximise this interaction.
  • lower modes are preferred, in particular modes which provide only a single node in the x and z dimensions (where x and z are transverse to the cavity length and y lies along the length of the cavity).
  • modes that provide two or more nodes along the length of the cavity i.e. the y dimension
  • a resonant mode providing two or more nodes is referred to as a "multi-node" pattern or mode. As discussed below in some methods the Applicant takes advantage of the structure of multi-node patterns to promote particular desired reactions.
  • the cavity 2 is designed to operate in TE1 1 1 or TM010 mode.
  • the nodes lie on a single node axis that passes down the centre line of the cavity. This is represented by pattern 60, which lies along the centre of the cavity and includes a series of nodes 61 and antinodes 62.
  • the microwave pattern in an empty ideal cavity is referred to as the "natural resonant mode”.
  • Figure 3A is an end view depicting the central position of the node 61 within the cavity 2.
  • the microwave pattern is perturbed by the presence in the cavity of the feed conduit and the feed material.
  • the resonant mode in the presence of feed conduit and feed material will be referred to as the "perturbed resonant mode".
  • the perturbation is believed to be created by contributions from the feed conduit and feed material, in particular from their conductivity, permittivity and permeability.
  • the Applicant believes that the complex components of the permittivity and permeability provide the most significant contribution.
  • These parameters, and therefore the perturbation vary with temperature. In a real world system with non-uniform materials these parameters also vary with time. These parameters also vary with changes in physical state. For example, water interacts strongly with microwave radiation at 2450MHz, but steam interacts weakly. Physical state is temperature and pressure dependent.
  • the perturbation results in a movement of the node axes away from the centre of the cavity cylinder. In some embodiments this movement may be in a direction towards or away from the waveguide. Without being bound by theory, the Applicant believes that this may be either a simple offset of the natural resonant mode, or may be a movement of the natural resonant mode towards a higher mode.
  • Figures 4 and 4A are views similar to Figures 3 and 3A showing the nodes of the perturbed resonant mode offset by a distance 65 from a central region marked by the dashed circle 66.
  • the feed tube 14 has also been offset from the centre of the cavity in order to align with the node axis. This offset is transverse to the length of the cavity, i.e. in the x or z dimension.
  • the offset may be achieved by offsetting the sleeves 9 and feed tube, or offsetting only the feed tube where the sleeve aperture is large enough to allow this.
  • the Applicant's cavity can be adapted to suit different feed materials by setting the offset at a suitable magnitude and allowing real time control of certain parameters.
  • An iterative approach may be used to determine the required offset.
  • a sample feedstock was created as a solid rod mimicking the properties of a proposed waste material. This feedstock was inserted into the cavity at an approximate expected offset based on first level modelling. The apparatus was switched on and run for a period of time to transfer energy to the sample feedstock. The apparatus was then switched off and the feedstock removed. Areas of the feedstock that had been strongly heated were discoloured.
  • an adjustment of the offset could be determined, or the information obtained could be used to adjust the model (in particular the permittivity and permeability values used in the model), with a new expected offset being obtained from the adjusted model.
  • a new sample feedstock was inserted with the adjusted offset and the process repeated until it was believed that the offset was correctly set to align the feed material with the perturbed nodes of the perturbed resonant mode.
  • the required offset is expected to be up to 1 8 mm, for a cavity operating at 2450Mhz and a 76mm diameter, or up to 60mm for a cavity operating at 915MHz with a diameter of 248mm.
  • the Applicant allows real time adjustment of one or more of: feed rate, power, offset and waveguide tuning, as will be described in detail below. In practice these adjustments allow for operation within a range of material parameters and maintain a high efficiency during operation, with the perturbed nodes aligned with the feed tube.
  • FIG 2 is a schematic diagram of a system including the energy transfer apparatus.
  • the apparatus may be substantially as described above with reference to Figure 1 , including a cavity 2, sleeves 9, waveguide 6 and feed tube 14.
  • a pump 20 is arranged to supply feed material from a source 21 to an inlet end of the feed tube 14.
  • the source 21 may supply feed material under pressure such that a separate pump 20 is not required.
  • a valve 22 may further control flow of feed material into the feed tube 14.
  • One or more further sources 23 may be provided for the introduction of other materials, such as catalysts, reactants or reaction suppressants, into the feed tube.
  • Each source 23 may have an associated pump and/or controllable valve 24 for controlling introduction of the other materials into the feed conduit.
  • the feed material and any other materials that may be mixed with it pass through the microwave cavity 2.
  • the properties of the output material may be monitored by a number of output sensors 27, 28.
  • the output sensors may include one or more temperature sensors, such as an optical pyrometer that is configured to take a reading from the outside of the feed tube.
  • the output sensors may also include one or more chemical sensors adapted to monitor the chemical make up of the output product, or to detect the presence or absence of a particular chemical in the output product. For example gas analyzers, quadrupole residual gas analysers, infra red gas monitors, mass flow detectors, electron capture detectors, mass spectrometers, FTIR spectrometers, hydrocarbon monitors or thermal conductivity detectors may be used, as appropriate for the particular application.
  • the output product passes to an outlet 30 and may be dealt with in any suitable manner for the application, such as by transmission to a packaging system, holding tank etc.
  • the output product may be a desired product to be retained and used or packaged, or it may be a waste product that has been treated in the apparatus such that it is less harmful or dangerous and can now be safely disposed of.
  • FIG. 2 also shows a microwave source 32, which provides microwave energy to the cavity 2 via waveguide 6.
  • Microwave energy may also pass from the cavity to the waveguide, or may be reflected back into the waveguide at the interface between the waveguide and cavity.
  • a directional isolator 33 is provided to remove microwave radiation that is travelling towards the source 32. This may be a three port microwave circulator (or cycler) in which energy is freely transmitted from the source 32 to the cavity 2, but energy travelling from the cavity towards the source is sent to a third port connected to a dead load. That energy is absorbed by the dead load and therefore removed from the waveguide 6.
  • Microwave sensors 35 are also connected to the waveguide 6 in order to monitor the microwave energy being transmitted from the source 32 towards the cavity 2 and also the microwave energy travelling towards the source 32.
  • the microwave sensors may be directional couplers connected to ferrite tile microwave detectors, or any other suitable detectors.
  • the cavity impedance may be variable dues to the variable nature of the feed material and, to some extent, the feed tube material.
  • a tuner 36 is mounted in the waveguide 6 in order to tune the impedance and therefore reduce the impedance mismatch.
  • the tuner 36 may be a three stub tuner. In one embodiment two stubs are fixed while the third is adjustable in real time by a suitable actuator controlled by a controller. Note that the reflected energy is not simply detected and the impedance mismatch minimised. The reflected radiation provides important information about reaction conditions in the cavity, and this information is used in order to provide improved performance.
  • an increase in reflected energy indicates an increased impedance mismatch.
  • the impedance of the waveguide will not have changed.
  • the increased mismatch therefore indicates an alteration in the impedance in the cavity. If the cavity has been up to temperature for some time, the contribution of the feed tube is unlikely to have changed, meaning that the impedance change is due to a changed contribution from the feed material. This may indicate an air bubble in the feed tube or simply a change in the constituents of the feed material.
  • the reflected energy provides information on the reaction rates or the degree to which the reaction is completed.
  • carbon is produced and the level of carbon in the feed tube will have an impact on the apparent cavity impedance.
  • the reflected energy therefore provides information on changes in the degree of completion of the pyrolysis reaction.
  • the reflected energy provides this information almost instantaneously, in contrast to the short delay that applies for the temperature and chemical detectors discussed above.
  • Temperature changes may also cause changes in the cavity impedance, as the permittivity, permeability and conductivity of the materials in the feed tube may vary with temperature.
  • a low level of reflected energy may indicate an efficient transfer of power to the feed material.
  • phase information can also be retrieved and may be interpreted to provide information on what is occurring in the cavity.
  • a detected impedance mismatch may be either positive or negative.
  • Phase information allows a determination to be made as to whether the mismatch is positive or negative and therefore of whether the apparent cavity impedance has increased or decreased. This in turn allows a determination to be made as to the change in the impedance contribution from the feed material, and depending on the application this will provide information on what is occurring within the feed tube.
  • the tuning of the tuner to eliminate the impedance mismatch is aided because it is known in which direction the tuning should be adjusted.
  • reaction conditions may be aided by knowledge of the reactions occurring or likely to occur within the feed tube.
  • This information may be stored in any suitable manner, for example in databases or lookup tables, or may be built into the control software.
  • This aspect of the system is also an important safety feature.
  • the reflection of a large amount of energy away from the cavity is ( 7potentially a significant safety problem. This may, for example, indicate a fault in the feed system resulting in the presence of a plug of air in the feed tube. This would cause a significant change in cavity impedance and low microwave absorption in the cavity. With continuing application of microwave power to the cavity this quickly creates large amounts of energy propagating in the waveguide and within the cavity.
  • the Applicant's controller can sense, via the microwave sensors 35, a sudden change of this type and reduce the microwave power or take other precautions as appropriate to ensure safe operation of the system.
  • the Applicant's system may also include an adjustable arrangement configured to alter the relative positions of the feed tube and the cavity. This may be achieved by keeping the feed tube fixed and moving the cavity.
  • the cavity may be fixed while the feed tube 14 is mounted to a moveable structure 37. Movement of the structure 37 is controlled by an actuator 38 such as a stepper motor or some other driver.
  • the sleeves 9 may remain fixed, with the bore through the sleeves being large enough to accommodate movement of the feed tube.
  • Figure 2 also shows a controller 40.
  • the controller 40 receives inputs from various sensors and controls the system in order to achieve desired heating or reaction conditions.
  • the controller 40 may receive information from one or more source sensors 41 over sensing lines 42. These may include one or more of: a level sensor, pressure sensor, temperature sensor, chemical sensors (e.g. a sensor to determine water content). These parameters enable the controller to determine properties of the feed material supplied by the source and to control the apparatus accordingly.
  • the controller controls the pump 20 over control line 44 and/or the valve 22 over control line 45. This enables the controller 40 to control a flow rate of feed material into the feed tube 14.
  • the controller also controls the ingress of other materials from sources 23, by control of the valves 24 over control lines 47.
  • sensors may be used to ensure that the amount of catalyst in the feed tube is at a desired level.
  • the controller may control the adjustment of feed tube position in the cavity by control of the actuator 38 over control line 48.
  • the controller 40 may control the microwave source's output power over control line 49.
  • the controller may control operation of the adjustable tuner 36 over control line 51 . This control may be in accordance with sensing information received from the directional microwave sensor 35 over sensor lines 52.
  • the controller may control the adjustable tuner 36 in order to minimise the level of microwave radiation travelling in the waveguide 6 away from the cavity 2.
  • the controller 40 may also receive sensing information from sensors 27, 28 over sensing lines 53, 54.
  • the sensed information can be used to maintain safety and to keep the apparatus operating within desired operating parameters.
  • the apparatus may be used to provide energy sufficient to heat the feed material to a certain temperature range. This may be a temperature necessary for sterilisation, or may be a temperature sufficient to cause a reaction (e.g. a pyrolysis reaction) to occur. It may be desirable to keep the temperature within both lower and upper limits.
  • the energy imparted to the feed material flowing through the feed tube will depend on the properties of the material, flow rate, the power output of the microwave source and the quality of alignment between the feed conduit and the nodes of the perturbed resonant mode pattern.
  • the temperature gain will depend on the energy transfer and the heat capacity of the feed material.
  • Initial feed rate and power values can be calculated based on the required temperature and estimated or measured material properties.
  • the temperature of the feed material can be indirectly measured using an optical pyrometer 27.
  • the optical pyrometer is mounted in a small sleeve similar to the sleeves 9 but of smaller diameter.
  • the pyrometer is directed into the centre of the cavity to measure the temperature of the feed conduit in the centre of the cavity.
  • the feed conduit is heated by the feed material flowing through it and its temperature is therefore indicative of the feed material temperature. If the temperature is too low, the feed rate may be slowed and/or the power of the source may be increased. If the temperature is too high, the feed rate may be increased and/or the power of the source may be decreased.
  • the Applicant's system may include one or more chemical sensors. Depending on the process involved, the presence of certain chemicals may indicate a complete or incomplete reaction has occurred, which may indicate that the reaction conditions are either satisfactory or need to be altered. Further, the presence of certain chemicals may indicate that an undesirable reaction has occurred, which may indicate that the reaction conditions need to be altered.
  • This sensor is also susceptible to a slight time lag, although a shorter time lag than the optical pyrometer.
  • the time lag for the pyrometer is 10 or more seconds, as opposed to around 1 second for the chemical sensor.
  • Blanket gases or reaction suppressant gases may be used.
  • nitrogen gas may be supplied to the feed tube.
  • Nitrogen has a high specific heat and therefore absorbs heat well, which is useful where second phase reactions are exothermic. Nitrogen can be used to control the heat output from these second phase reactions. Nitrogen can also be used to suppress fire and to rapidly close down the reaction if necessary for safety reasons.
  • Steam may also be used as a blanket gas. Steam is particularly useful where the final reaction temperature is above 600°C and the steam produces hydrogen by the water gas reaction. Pyrolysis gas products containing the hydrogen can then be used as the raw material entrainment gas where hydrogenation is one of the low energy catalysed reactions.
  • Blanket gases may also tend to reduce the sensing time lags for the chemical sensors, because they tend to carry reaction product gases more quickly to the sensors.
  • gas mixers may be used to mix gas into the paste.
  • microwave sensors in the waveguide function as discussed above to provide information on reaction conditions within the cavity, without any significant time lag.
  • the information from the various sources can be gathered and used to optimise the reaction conditions within the feed tube.
  • FIG. 5 shows a further embodiment in which a higher order resonant mode is used.
  • this embodiment there are two node axes running the length of the cavity and two feed tubes 14, 14' are mounted such that one feed tube is aligned with each set of nodes 60, 60'.
  • Each feed tube is mounted in a set of sleeves 9, 9'.
  • Each tube is offset from a natural mode axis to align with the perturbed nodes, as discussed above.
  • any suitable resonant mode may be used. However, correct alignment is likely to be more difficult for higher modes, and for this reason the TM010 or TE 1 1 1 mode is preferred.
  • the correct alignment of the feed tube with the perturbed nodes of the perturbed resonant mode provides improved transfer of energy to material flowing through the feed tube.
  • the feed tube is preferably arranged to pass through two or more of these nodes, ideally all of these nodes, to obtain the greatest possible energy transfer.
  • the Applicant's apparatus results in improved efficiency over prior systems, with efficiency now over 85% at 2450MHz and over 90% at 91 5MHz.
  • the apparatus may be used in any application where transfer of energy to a continuous flow of material is required. Examples include: pyrolysis, heating or drying apparatuses, and chemical reactors, in particular reactors for suitable endothermic chemical reactions.
  • the controller is configured to control microwave power for safety purposes, particularly where there is a sudden change in the level of reflected microwave energy in the waveguide.
  • the controller may operate to keep the feed material within a certain temperature range, or may operate to maintain desired reaction conditions to produce desired reaction products.
  • the output of the various sensors may be used to assist with interpretation of what is happening in the cavity. For example, an increase in reflected energy in the waveguide can be interpreted with help from temperature or reaction product information.
  • reaction suppressant such as an inert gas
  • the microwave isolator and control mechanisms associated with reflected energy in the waveguide help to prevent the energy levels from rising beyond safe limits or from affecting the microwave source.
  • the Applicant's apparatus may be configured to provide two or more nodes in sequence.
  • the resonant mode pattern can be controlled to some extent by the positioning of the waveguide interface along the length of the cavity.
  • Figure 6 shows a computer model of the resonant mode in one embodiment.
  • a maximum node ie a node with maximum energy transfer to the feed substance
  • Other nodes, arranged along the length of the cavity will have lesser magnitudes or intensities (i.e. level of energy transfer to the feed substance) than the maximum node, with their magnitudes or intensities generally falling off along the length of the cavity. There is therefore a maximum energy transfer to the feed substance at the maximum node, and a lesser energy transfer to the feed substance at other nodes.
  • a desired chemical process may include first and second reaction stages.
  • a first stage of the reaction may have a first activation energy Ei .
  • a second stage of the reaction may have a second activation energy E2, with E2 greater than Ei .
  • the reaction can be performed in two stages as follows.
  • the waveguide is positioned along the length of the cavity such that a first node is positioned near an input end of the cavity.
  • a second node, the maximum node is positioned further along the length of the cavity. In use, the feed substance will pass from the input end of the cavity to the first node.
  • Microwave power and other cavity parameters may be controlled such that the energy provided at the first node is sufficient to provide the activation energy Ei and the first reaction stage will therefore be promoted, forming a partially reacted feed substance. If necessary the microwave power and other cavity parameters may be controlled such that the energy provided at the first node is less than the activation energy E2. This ensures that second stage reactions do not proceed in the first node.
  • the partially reacted feed substance will then pass to the second (maximum) node.
  • Microwave power and other cavity parameters may be controlled such that the energy provided at the second node is sufficient to provide the activation energy E2 and the second reaction stage will therefore be promoted.
  • This method may be extended to any number of reaction stages, with the substance passing through the feed tube being subjected to ever increasing energy levels that sequentially energise different reaction stages, each stage including one or more chemical reactions.
  • the feed substance may be passed through the feed tube in any suitable form.
  • the material to be treated may be extruded together with any required catalysts into a solid plastic rod (for example by a plastic screw extruder) and the rod passed through the feed tube.
  • the extruder may be mounted near the cavity in order to feed the rod directly into the reaction tube.
  • the rod may be around 7mm in diameter for a 2450 MHz cavity, or around 19mm for a 91 5 MHz cavity.
  • the rods may be fed into the reaction tube by any suitable system, including cooperating friction wheels or the like, driven by an electric motor or any other suitable power source.
  • the speed or rate at which the material is fed into the reaction tube is preferably adjustable and may be manually or automatically controlled.
  • the raw product may be solid, liquid or gas as appropriate for the application.
  • the feed substance (including any required catalysts etc) may be passed through an airlock system into the reaction tube in order to exclude atmospheric gases from the reaction tube.
  • the airlock may be a cavity with an inlet opening having a seal dimensioned to seal against an outer surface of the substance rod.
  • An outlet from the cavity may lead directly to the reaction tube, with appropriate seals sealing the connection.
  • a gas may be fed into the cavity at sufficient pressure to assist in sealing of the cavity and in exclusion of atmospheric gases.
  • the gas is preferably one that will not have any effect on the reaction if it passes into the reaction tube. In many embodiments the gas should be oxygen free. Inert gases may be preferred in some embodiments.
  • a mixture of 1 0% (w/w) PWdC, 10% (w/w) EVA, 75% (w/w) LLDPE and 5% (w/w) carbon was extruded as a rod of 20 mm diameter.
  • the rod was fed through the length of the elongated resonant cavity of the apparatus at a rate of 28 mm/min.
  • the cavity was operated at a frequency of 2450 MHz and power of 1 kW.
  • Greater than 95% pyrolysis was achieved at a temperature of 180°C based on the conversion of the mixture to volatile products and carbonaceous residue at this temperature.
  • HCI gaseous hydrogen chloride
  • HCVI gaseous hydrogen chloride
  • Comparative Example III The resonant cavity was operated at a frequency of 2450 MHz. A blend of PCB treated wood and 5% (w/w) carbon was subjected to pyrolysis at temperatures up to 400°C. No de-chlorination of PCB could be detected.
  • the resonant cavity was operated at a frequency of 2450 MHz.
  • a blend of PCB treated wood and 5% (w/w) titanium dioxide-magnetite was subjected to pyrolysis at 300°C. No chlorinated organic substances were detectable in the liquid products of pyrolysis.
  • the resonant cavity was operated at a frequency of 2450 MHz at a temperature of 350°C.
  • Organic substances were subjected to pyrolysis in the cavity under an atmosphere of 30% hydrogen in nitrogen. Greater than 95% pyrolysis of a mixture of 10% (w/w) PVdC, 10% (w/w) EVA and 70% (w/w) LLDPE was achieved when blended with 10% (w/w) of a mixture of in equal parts by weight of carbon treated with nickel and titanium dioxide- magnetite.
  • No chlorinated organic substances such as polychlorinated di- benzyl dioxins (PCDD) and polychlorinated di-benzyl furans (PCDF) were detected in the volatile products of pyrolysis.
  • PCDD polychlorinated di- benzyl dioxins
  • PCDF polychlorinated di-benzyl furans
  • the apparatus and methods are applicable to the processing of waste.
  • Friar and Henare (201 1 ) Improvements in chemical reactions International Publication No. WO 201 1/045638 A2.

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  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
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Abstract

L'invention concerne un appareil de transfert d'énergie comprenant une cavité à micro-ondes pour le transfert d'énergie à des substances avancées dans la cavité. Divers procédés de réaction ou de chauffage peuvent être mis en œuvre en utilisant la cavité, comprenant un procédé de pyrolyse de substances organiques, comme des substances organiques polychlorées, sous la forme d'un processus continu.
PCT/NZ2012/000210 2011-11-11 2012-11-12 Appareil à micro-ondes et procédés associés WO2013070095A1 (fr)

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AU2012202004A AU2012202004A1 (en) 2012-04-04 2012-04-04 Microwave energy transfer apparatus

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US9700852B2 (en) 2012-08-28 2017-07-11 So Spark Ltd. System, method and capsules for producing sparkling drinks
US10143977B2 (en) 2012-08-28 2018-12-04 So Spark Ltd. System method and capsules for producing sparkling drinks
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