US20060237300A1 - Treatment of granular solids in a fluidized bed with microwaves - Google Patents

Treatment of granular solids in a fluidized bed with microwaves Download PDF

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Publication number
US20060237300A1
US20060237300A1 US10/540,433 US54043303A US2006237300A1 US 20060237300 A1 US20060237300 A1 US 20060237300A1 US 54043303 A US54043303 A US 54043303A US 2006237300 A1 US2006237300 A1 US 2006237300A1
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Prior art keywords
fluidized
wave guide
bed
bed reactor
reactor
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US10/540,433
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English (en)
Inventor
Michael Stroder
Nikola Anastasijevic
Thorsten Gerdes
Monika Willert-Porada
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Outokumpu Oyj
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Outokumpu Oyj
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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
    • H05B6/80—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
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
    • B01J8/1872—Details of the fluidised bed reactor
    • 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
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
    • B01J8/24—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles according to "fluidised-bed" technique
    • B01J8/36—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles according to "fluidised-bed" technique with fluidised bed through which there is an essentially horizontal flow of particles
    • 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
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
    • B01J8/24—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles according to "fluidised-bed" technique
    • B01J8/38—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles according to "fluidised-bed" technique with fluidised bed containing a rotatable device or being subject to rotation or to a circulatory movement, i.e. leaving a vessel and subsequently re-entering it
    • B01J8/384—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles according to "fluidised-bed" technique with fluidised bed containing a rotatable device or being subject to rotation or to a circulatory movement, i.e. leaving a vessel and subsequently re-entering it being subject to a circulatory movement only
    • B01J8/388—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles according to "fluidised-bed" technique with fluidised bed containing a rotatable device or being subject to rotation or to a circulatory movement, i.e. leaving a vessel and subsequently re-entering it being subject to a circulatory movement only externally, i.e. the particles leaving the vessel and subsequently re-entering it
    • 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
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
    • B01J8/24—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles according to "fluidised-bed" technique
    • B01J8/42—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles according to "fluidised-bed" technique with fluidised bed subjected to electric current or to radiations this sub-group includes the fluidised bed subjected to electric or magnetic fields
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B1/00—Preliminary treatment of ores or scrap
    • C22B1/02—Roasting processes
    • C22B1/10—Roasting processes in fluidised form
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B11/00—Obtaining noble metals
    • C22B11/02—Obtaining noble metals by dry processes
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F26—DRYING
    • F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
    • F26B3/00—Drying solid materials or objects by processes involving the application of heat
    • F26B3/02—Drying solid materials or objects by processes involving the application of heat by convection, i.e. heat being conveyed from a heat source to the materials or objects to be dried by a gas or vapour, e.g. air
    • F26B3/06—Drying solid materials or objects by processes involving the application of heat by convection, i.e. heat being conveyed from a heat source to the materials or objects to be dried by a gas or vapour, e.g. air the gas or vapour flowing through the materials or objects to be dried
    • F26B3/08—Drying solid materials or objects by processes involving the application of heat by convection, i.e. heat being conveyed from a heat source to the materials or objects to be dried by a gas or vapour, e.g. air the gas or vapour flowing through the materials or objects to be dried so as to loosen them, e.g. to form a fluidised bed
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F26—DRYING
    • F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
    • F26B3/00—Drying solid materials or objects by processes involving the application of heat
    • F26B3/02—Drying solid materials or objects by processes involving the application of heat by convection, i.e. heat being conveyed from a heat source to the materials or objects to be dried by a gas or vapour, e.g. air
    • F26B3/06—Drying solid materials or objects by processes involving the application of heat by convection, i.e. heat being conveyed from a heat source to the materials or objects to be dried by a gas or vapour, e.g. air the gas or vapour flowing through the materials or objects to be dried
    • F26B3/08—Drying solid materials or objects by processes involving the application of heat by convection, i.e. heat being conveyed from a heat source to the materials or objects to be dried by a gas or vapour, e.g. air the gas or vapour flowing through the materials or objects to be dried so as to loosen them, e.g. to form a fluidised bed
    • F26B3/084—Drying solid materials or objects by processes involving the application of heat by convection, i.e. heat being conveyed from a heat source to the materials or objects to be dried by a gas or vapour, e.g. air the gas or vapour flowing through the materials or objects to be dried so as to loosen them, e.g. to form a fluidised bed with heat exchange taking place in the fluidised bed, e.g. combined direct and indirect heat exchange
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F26—DRYING
    • F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
    • F26B3/00—Drying solid materials or objects by processes involving the application of heat
    • F26B3/32—Drying solid materials or objects by processes involving the application of heat by development of heat within the materials or objects to be dried, e.g. by fermentation or other microbiological action
    • F26B3/34—Drying solid materials or objects by processes involving the application of heat by development of heat within the materials or objects to be dried, e.g. by fermentation or other microbiological action by using electrical effects
    • F26B3/343—Drying solid materials or objects by processes involving the application of heat by development of heat within the materials or objects to be dried, e.g. by fermentation or other microbiological action by using electrical effects in combination with convection
    • 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
    • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00008—Controlling the process
    • B01J2208/00017—Controlling the temperature
    • B01J2208/00106—Controlling the temperature by indirect heat exchange
    • B01J2208/00115—Controlling the temperature by indirect heat exchange with heat exchange elements inside the bed of solid particles
    • B01J2208/00141—Coils
    • 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
    • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00008—Controlling the process
    • B01J2208/00017—Controlling the temperature
    • B01J2208/00433—Controlling the temperature using electromagnetic heating
    • B01J2208/00442—Microwaves
    • 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
    • B01J2219/1287—Features relating to the microwave source
    • B01J2219/129—Arrangements thereof
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B5/00—General methods of reducing to metals
    • C22B5/02—Dry methods smelting of sulfides or formation of mattes
    • C22B5/12—Dry methods smelting of sulfides or formation of mattes by gases
    • C22B5/14—Dry methods smelting of sulfides or formation of mattes by gases fluidised material

Definitions

  • This invention relates to a method for the thermal treatment of granular solids in a fluidized bed which is located in a fluidized-bed reactor, wherein microwave radiation is fed into the fluidized-bed reactor through at least one wave guide, and to a corresponding plant.
  • microwave source there are several possibilities for coupling a microwave source to fluidized-bed reactors. These include for instance an open wave guide, a slot antenna, a coupling loop, a diaphragm, a coaxial antenna filled with gas or another dielectric, or a wave guide occluded with a microwave-transparent substance (window).
  • the type of decoupling the microwaves from the feed conduit can be effected in different ways.
  • microwave energy can be transported in wave guides free of loss.
  • the wave guide cross-section is obtained as a logical development of an electric oscillating circuit comprising coil and capacitor towards very high frequencies.
  • Theoretically, such oscillating circuit can likewise be operated free of loss.
  • the coil of an electric oscillating circuit becomes half a winding, which corresponds to the one side of the wave guide cross-section.
  • the capacitor becomes a plate capacitor, which likewise corresponds to two sides of the wave guide cross-section.
  • an oscillating circuit loses energy due to the ohmic resistance in coil and capacitor.
  • the wave guide loses energy due to the ohmic resistance in the wave guide wall.
  • Energy can be branched off from an electric oscillating circuit by coupling a second oscillating circuit thereto, which withdraws energy from the first one.
  • a second wave guide to a first wave guide energy can be decoupled from the same (wave guide transition).
  • the microwave energy in a wave guide is enclosed by the electrically conductive walls.
  • wall currents are flowing, and in the wave guide cross-section an electromagnetic field exists, whose field strength can be several 10 KV per meter.
  • an electrically conductive antenna rod When an electrically conductive antenna rod is put into the wave guide, the same can directly dissipate the potential difference of the electromagnetic field and with a suitable shape also emit the same again at its end (antenna or probe decoupling).
  • An antenna rod which enters the wave guide through an opening and contacts the wave guide wall at another point can still directly receive wall currents and likewise emit the same at its end.
  • the wave guide is shut off by a shorting plunger behind the antenna coupling, the entire energy can be diverted from the wave guide into the antenna in this case as well.
  • Microwave radiation can be conducted in electrically conductive hollow sections of all kinds of geometries, as long as their dimensions do not fall below certain minimum values.
  • the exact calculation of the resonance conditions involves rather complex mathematics, as the Maxwell equations (unsteady, nonlinear differential equations) must ultimately be solved with the corresponding marginal conditions.
  • the equations can be simplified to such an extent that they can be solved analytically and problems as regards the design of wave guides become clearer and are easier to solve. Therefore, and due to the relatively easy production, only rectangular wave guides or round wave guides are used industrially, which are also preferably used in accordance with the invention.
  • the chiefly used rectangular wave guides are standardized in the Anglo-Saxon literature.
  • a method for the thermal treatment of granular solids is known from U.S. Pat. No. 5,972,302, wherein sulfidic ore is subjected to an oxidation supported by microwaves.
  • This method is chiefly concerned with the calcination of pyrite in a fluidized bed, wherein the microwaves introduced into the fluidized bed promote the formation of hematite and elementary sulfur and suppress the formation of SO 2 .
  • a stationary fluidized bed which Is directly irradiated by the microwave source disposed directly above the same.
  • the microwave source or the entrance point of the microwaves necessarily gets in contact with the gases, vapors and dusts ascending from the fluidized bed.
  • EP 0 403 820 B1 describes a method for drying substances in a fluidized bed, wherein the microwave source is disposed outside the fluidized bed and the microwaves are introduced into the fluidized bed by means of a wave guide.
  • the microwave source is disposed outside the fluidized bed and the microwaves are introduced into the fluidized bed by means of a wave guide.
  • there are also dust deposits in the wave guide which absorb part of the microwave radiation and can damage the microwave source. This can be avoided by microwave-transparent windows, which occlude the wave guide between the reactor and the microwave source. In this case, however, deposits on the window lead to an impairment of the microwave radiation.
  • this object is substantially solved in a method as mentioned above in that the irradiation angle of the microwaves is inclined by an angle of 10° to 50°, particularly preferably, however, between 10° and 20°, with respect to the principal axis of the fluidized-bed reactor.
  • the irradiation angle ⁇ can also be variably adjustable.
  • Electromagnetic waves are transverse waves, i.e. have a polarizing direction, the direction of the electric field strength being parallel to the transmitter dipole, the direction of the magnetic excitation vertical thereto.
  • the degree of reflection must be minimized. The degree of reflection is known to depend on the angle of incidence, the refractive index of the substance to be excited, and on the polarizing direction.
  • the substances to be excited in the fluidized bed are ores, recycling substances or waste substances, which either unevenly lie on a grid in the fluidized bed or circulate with introduced gas in the reactor space, there is no distinct surface on which the microwave rays impinge.
  • the reflected microwaves form standing waves of multiple modes in the reactor space. These modes are also obtained in the case of microwaves from only one microwave source, as the microwaves are reflected at the wall of the reactor in various directions. These microwaves reinforce each other by increasing the amplitude in some regions, and cancel each other again in other regions. This produces a multitude of standing waves. It was surprisingly found out that in particular with an irradiation angle of the microwaves of 10 to 20 degrees with respect to the principal axis of the reactor the smallest reflection and thus the highest efficiency can be achieved. By principal axis of the reactor there is in particular meant the vertical axis of symmetry. The reflection onto the microwave source also is smallest at the same time. For protection, the microwave source also is disposed outside the stationary or circulating fluidized bed, the microwave radiation being fed into the fluidized-bed reactor through at least one wave guide.
  • a gas stream is additionally fed into the fluidized-bed reactor through the wave guide, which gas stream is also used for microwave irradiation. Coupling the microwave radiation and at the same time the secondary stream under an angle of 10° up to in particular 20° into the fluidized-bed reactor turned out to be particularly favorable, as in this angular range the returning microwave performance is minimal on the one hand and on the other hand no dust deposits are observed in the wave guide. Hence, the heating efficiency and the operational safety are highest in this range. In dependence on the properties of the fluidized bed, however, irradiation angles between 200 and 50° may be expedient in terms of apparatus.
  • microwave-transparent windows in the wave guide for shielding the microwave source can therefore be omitted.
  • the same involve the problem that deposits of dust or other solids on the window can impair and partly absorb the microwave radiation. Therefore, the open wave guides in accordance with the invention are particularly advantageous.
  • the thermal treatment can not only be effected in a stationary, but also in a circulating fluidized bed, wherein the solids circulate continuously between a fluidized-bed reactor, a solids separator connected with the upper region of the fluidized-bed reactor and a return conduit connecting the solids separator with the lower region of the fluidized-bed reactor.
  • the amount of solids circulating per hour is at least three times the amount of solids present in the fluidized-bed reactor.
  • Suitable microwave sources i.e. sources for the electromagnetic waves, include e.g. a magnetron or a klystron. Furthermore, high-frequency generators with corresponding coils or power transistors can be used.
  • the frequencies of the electromagnetic waves proceeding from the microwave source usually lie in the range from 300 MHz to 30 GHz.
  • the ISM frequencies 435 MHz, 915 MHz and 2.45 GHz are used. Expediently, the optimum frequencies are determined for each application in a trial operation.
  • the wave guide wholly or largely consists of electrically conductive material, e.g. copper.
  • the length of the wave guide lies in the range from 0.1 to 10 m.
  • the wave guide may be straight or curved. There are preferably used sections of round or rectangular cross-section, the dimensions being in particular adjusted to the frequency used.
  • the temperatures in the fluidized bed lie for instance in the range from 150 to 1200° C., and it may be recommended to introduce additional heat into the fluidized bed, e.g. through indirect heat exchange.
  • insulated sensing elements, radiation pyrometers or fiber-optic sensors can be used.
  • the gas velocities in the wave guide are adjusted such that the Particle-Froude-Numbers in the wave guide lie in the range between 0.1 and 100.
  • gas serving as purge gas flows through the wave guide.
  • Solid particles can for instance be dust particles present in the reactor or also the treated solids.
  • Process gases are obtained in the processes which take place in the reactor.
  • the density ratio of the entering solid particles or process gases to the purge gas is considered in accordance with the invention when adjusting the gas velocities, which ratio, apart from the velocity of the purge gas stream, is decisive for the question whether or not the purge gas stream can entrain the entering particles. Substances can thereby be prevented from penetrating into the wave guide.
  • a Particle-Froude-Number between 2 and 30 is preferred.
  • the granular solids to be treated by the method in accordance with the invention can for instance be ores and in particular sulfidic ores, which are prepared e.g. for recovering gold, copper or zinc. Furthermore, recycling substances, e.g. zinc-containing processing oxide or waste substances, can be subjected to the thermal treatment in the fluidized bed. If sulfidic ores, such as e.g. auriferous arsenopyrite, are subjected to the method, the sulfide is converted to oxide, and with a suitable procedure there is preferably formed elementary sulfur and only small amounts of SO 2 .
  • the method of the invention favorably loosens the structure of the ore, so that the subsequent gold leaching leads to improved yields.
  • the arsenic iron sulfide (FeAsS) preferably formed by the thermal treatment can easily be disposed of.
  • the solids to be treated at least partly absorb the electromagnetic radiation used and thus heat the bed. It was surprisingly found out that in particular material treated at high field strengths can be leached more easily. Frequently, other technical advantages can be realized as well, such as reduced retention times or a decrease of the required process temperatures.
  • the solids can also be passed through at least two succeeding fluidized-bed reactors, for instance two turbulence chambers separated from each other by means of weirs or partitions, in which the stationary fluidized beds are disposed and into which electromagnetic waves are fed, which are coming from wave guides.
  • the solids can move as migrating fluidized-bed from one fluidized-bed reactor into the adjacent fluidized-bed reactor.
  • One variant consists in that between two turbulence chambers of the two adjacent fluidized-bed reactors an intermediate chamber is disposed, which is connected with the turbulence chambers and contains a fluidized bed of granular solids, the intermediate chamber having no wave guide associated thereto.
  • Another variant of the method of the invention consists in that for separating the two turbulence chambers a partition is used, which has the opening in the bottom region.
  • the operating conditions in particular temperature, composition of the fluidizing gas, energy input and/or fluidization velocity, can be predetermined differently for each of a plurality of fluidized-bed reactors.
  • the solids thus can for instance first be passed through a preheating chamber upstream of the first fluidized bed.
  • a cooling chamber downstream of the last fluidized bed serving the thermal treatment a cooling chamber can be provided for cooling the solid product.
  • a plant in accordance with the invention includes a fluidized-bed reactor, a microwave source disposed outside the fluidized-bed reactor, and a wave guide for feeding the microwave radiation into the fluidized-bed reactor, the wave guide being inclined by an angle of 10° to 500, in particular 10° to 20°, with respect to the principal axis of the fluidized-bed reactor.
  • FIG. 1 shows the thermal treatment of granular solids in a stationary fluidized bed in a schematic representation
  • FIG. 2 shows a method variant with a circulating fluidized bed
  • FIGS. 3, 4 , 5 show method variants with a plurality of stationary fluidized beds.
  • FIG. 1 shows a plant for performing the method in accordance with the invention for the thermal treatment of granular solids in a stationary fluidized layer 3 which is also referred to as fluidized bed.
  • the plant includes a fluidized-bed reactor 1 , into which granular solids to be treated are introduced through a conduit 2 .
  • the solids form a stationary fluidized bed 3 which is traversed by a fluidizing gas, e.g. air.
  • a fluidizing gas e.g. air
  • the fluidizing gas is passed from below through a gas distributor 4 into the fluidized bed 3 .
  • an open wave guide 5 which leads to a microwave source 7 , is connected to the chamber with the stationary fluidized bed 3 .
  • the wave guide 5 is inclined by an angle ⁇ of 10° to 20° with respect to the vertical principal axis 11 of the fluidized-bed reactor 1 .
  • the electromagnetic waves proceeding from the microwave source 7 are passed through the wave guide 5 and fed into the chamber of the fluidized-bed reactor 1 . They at least partly contribute to the heating of the fluidized bed 3 . Furthermore, purge gas, e.g. air or nitrogen, is laterally fed into the wave guide 5 through a conduit 6 , which purge gas flows on into the fluidized-bed reactor and prevents the ingress of dust or process gases from the chamber with the stationary fluidized bed 3 into the wave guide 5 . In this way, the microwave source 7 is protected against being damaged, and at the same time microwave-absorbing soil deposits in the wave guide 5 are prevented without the open wave guide 5 having to be closed by a microwave-transparent window. By means of the angle of inclination, reflections of the microwaves fed into the fluidized-bed reactor 1 are reduced considerably, so that the electromagnetic radiation can better be absorbed by the solids and the efficiency of the plant and of the method is increased.
  • purge gas e.g. air or nitrogen
  • the stationary fluidized bed 3 can additionally be heated by a heat exchanger 8 disposed in the fluidized bed 3 .
  • Gases and vapors formed leave the chamber of the fluidized-bed reactor 1 through a conduit 9 and are supplied to a non-illustrated cooling and dedusting known per se.
  • the treated granular solids are withdrawn from the fluidized-bed reactor 1 through the discharge conduit 10 .
  • the fluidized-bed reactor 1 constitutes a reactor with a circulating fluidized bed (fluidized layer).
  • the solids to be treated are introduced into the fluidized-bed reactor 1 via conduit 2 and entrained by fluidizing gas introduced into the fluidized-bed reactor 1 , whereby the circulating fluidized layer is formed.
  • the solids then are at least partly discharged from the fluidized-bed reactor 1 along with the gas through a duct 18 and introduced into a solids separator 12 .
  • the solids separated therein are at least partly recirculated through a return conduit 13 into the lower region of the circulating fluidized bed of the fluidized-bed reactor 1 . Part of the solids can also be discharged through the discharge conduit 14 .
  • Coarse solids which are deposited at the bottom of the fluidized-bed reactor 1 , can be removed from the reactor 1 through an outlet conduit 15 .
  • the fluidizing gas for forming the circulating fluidized bed e.g. air
  • the fluidizing gas for forming the circulating fluidized bed e.g. air
  • the fluidizing gas for forming the circulating fluidized bed e.g. air
  • the fluidizing gas for forming the circulating fluidized bed e.g. air
  • the fluidizing gas for forming the circulating fluidized bed e.g. air
  • a wave guide 5 connects a microwave source 7 with the chamber of the fluidized-bed reactor 1 , through which wave guide microwaves are fed into the microwave reactor 1 for heating the granular solids as in the plant in accordance with FIG. 1 .
  • purge gas from a secondary gassing 6 flows through the wave guide 5 , in order to avoid the ingress of dirt as well as deposits in the wave guide 5 .
  • the wave guide 5 is inclined by an angle ⁇ of 10° to 20° with respect to the principal axis 11 of the fluidized-bed reactor 1 , in order to minimize reflections of the irradiated microwaves at the solids and in conjunction with the gas stream avoid dust deposits in the wave guide 5 .
  • the microwave source 7 is disposed behind a bend of the wave guide 5 , in which the same is bent with respect to its longitudinal axis by about the angle ⁇ .
  • the secondary gassing 6 connected to a non-illustrated ring conduit substantially axially meets the wave guide 5 in this bend.
  • the inner region of the chamber can again be provided with one or more heat exchangers for additionally heating the granular solids, which was not represented in FIG. 2 for a better clarity.
  • Dust-laden gas leaves the solids separator 12 through conduit 9 and is first cooled in a waste heat boiler 16 , before it is passed through a dedusting 17 . Separated dust can either be removed from the process or be recirculated to the chamber of the fluidized-bed reactor 1 through a non-illustrated conduit.
  • two stationary fluidized-bed reactors 1 and 1 a are arranged in series, an intermediate chamber 1 c being located between the chambers of the two reactors 1 and 1 a .
  • the solids form a stationary fluidized bed 3 , 3 a , which is traversed by fluidizing gas.
  • the fluidizing gas for each chamber is supplied through a separate conduit 4 a .
  • the granular solids to be treated enter the first fluidized-bed reactor 1 through conduit 2 , and completely treated solids leave the second fluidized-bed reactor 1 a through the discharge conduit 10 . From the upper region of the chamber of the first reactor 1 a first wall 19 extends downwards.
  • wave guides 5 with purge air conduits 6 and microwave sources 7 are each connected to the chambers of the two reactors 1 and 1 a , which wave guides are inclined by an angle ⁇ between 10° and 20° against the vertical principal axis 11 .
  • the principal axes of the reactors 1 and 1 a are each aligned vertically and disposed in parallel, so that in the drawing merely one principal axis is shown.
  • the irradiation angle ⁇ in the first reactor 1 is different from the irradiation angle ⁇ in the second reactor 1 a .
  • This is in particular expedient when for instance microwaves of different frequencies are irradiated into the various chambers.
  • the two irradiation angles ⁇ are equal for both reactors 1 , 1 a .
  • heat exchanging elements 8 may be arranged in addition.
  • the gas space 22 above the fluidized bed 3 of the first fluidized-bed reactor 1 is separated from the gas space 23 , which belongs to the chamber of the second reactor 1 a and the intermediate chamber 1 c , by the vertical wall 19 .
  • the gas spaces 22 , 23 separate gas outlet conduits 9 and 9 a exist.
  • different conditions can be maintained in the chambers of the reactors 1 and 1 a , in particular different temperatures can exist or different fluidizing gases can be supplied through separate gas supply conduits 4 a .
  • the two microwave sources 7 can be designed differently and perform different functions. In particular, microwaves of different frequency or energy can be generated and be introduced through the wave guide 5 .
  • two stationary fluidized-bed reactors 1 and 1 a without intermediate chamber are arranged directly succeeding each other, a partition 19 being disposed between the two.
  • the solids form a stationary fluidized bed 3 , 3 a , which is fluidized by fluidizing gas from a plurality of conduits 4 a disposed one beside the other.
  • the granular solids to be treated are supplied to the first fluidized-bed reactor 1 through conduit 2 , and the treated solids leave the fluidized-bed reactor 1 a through the discharge conduit 10 .
  • a first wall 19 extends downwards, which does, however, not extend down to the ground, so that in the bottom region an opening 20 is left, through which solids from the first fluidized bed 3 can get into the fluidized bed 3 a of the second fluidized-bed reactor 1 a .
  • Waveguides 5 which are connected to the microwave sources 7 , each extend to the two chambers of the reactors 1 and 1 a . According to the principle described already in the previous embodiments, microwaves are fed into the two reactors 1 , 1 a through these open wave guides, in order to heat the solids to be treated, which absorb the microwave radiation, and reach the necessary process temperatures.
  • the wave guides 5 are again inclined by their respective irradiation angles ⁇ between 10° and 20° against the principal axes 11 of the two reactors 1 , 1 a .
  • purge gas at the same time flows into the wave guides 5 through purge air conduits 6 , in order to avoid deposits in said wave guides.
  • heat exchanging elements 8 may be arranged in addition.
  • the gas space 22 above the fluidized bed 3 of the first fluidized-bed reactor 1 is separated from the gas space 23 , which belongs to the chamber of the second reactor 1 a , by the vertical wall 19 .
  • different conditions can be maintained in the various reactor chambers 1 and 1 a , in particular the temperatures or the gas phase composition can be different.
  • Different fluidizing gases can also be supplied through the respective conduits 4 a .
  • the two microwave sources 7 can be designed differently and perform different functions.
  • the solids to be treated which are supplied via conduit 2 , first enter an antechamber 31 and flow through a first intermediate chamber 32 into the first fluidized-bed reactor 1 .
  • the solids then are discharged from the same to flow through a second intermediate chamber 1 c into the second fluidized-bed reactor 1 a and finally through the third intermediate chamber 33 into a cooling chamber 34 , before the treated and cooled solids are withdrawn through the discharge conduit 10 .
  • Wave guides 5 with associated non-illustrated microwave sources each open into the chambers of the fluidized-bed reactors 1 and 1 a , in order to feed microwaves into the reactors 1 and 1 a according to the above-described principle.
  • the wave guides are inclined at an angle ⁇ of 10° to 20° with respect to the principal axis 11 of the fluidized-bed reactors 1 , 1 a .
  • All chambers include stationary fluidized beds, to which fluidizing gas is supplied through separate gas supply conduits 4 a for each chamber. The exhaust gases are discharged through corresponding conduits 9 .
  • the fluidized bed includes a cooling means 35 for an indirect heat exchange, whose cooling fluid, e.g. cooling water, is heated in the cooling means 35 and then supplied through conduit 36 to the heat exchanger 37 in the preheating chamber 31 . There, the cooling fluid releases part of its heat to the solids in the fluidized bed disposed there, whereby a very economic utilization of heat is achieved.
  • a cooling fluid e.g. cooling water
  • the microwave source 7 in accordance with the invention is disposed outside the stationary or circulating fluidized bed 3 , 3 a and the fluidized-bed reactors 1 , 1 a .
  • the microwave radiation is fed into the fluidized-bed reactor 1 , 1 a through at least one open wave guide 5 , the irradiation angle of the microwaves being inclined by an angle of 10° to 50°, preferably 10° to 20°, with respect to the principal axis 11 of the respective fluidized-bed reactor 1 , 1 a.
  • the following Table indicates typical method parameters for a calcination of gold ore.
  • the microwave frequency is about 915 MHz in the indicated example.
  • without microwave with microwave Unit Inlet Outlet Inlet Outlet Diameter of the CFB- mm 200 200 reactor of FIG. 2 kW 0 2 Installed microwave kg/h 150 195 performance Gold ore feed ° C. 350 250 Primary air Nm 3 /h 30 30 kg/h 0.80 0.77 Oil consumption: ° C. 525 425 Secondary air Nm 3 /h 24 24 kg/h 140 182 Melting loss Calcination gas, total Nm 3 /h 58 59 Flow rate ° C. 700 600 Temperature Composition, dry vol-% 18.7 23.3 CO 2 vol-% 75.3 74.3 N 2 vol-% 5.9 2.4 O 2 ppV 220 134.1 SO 2
  • the plant capacity can be increased particularly with reduced emissions by using microwaves which are irradiated under an angle of inclination of 15°.

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US10/540,433 2002-12-23 2003-11-25 Treatment of granular solids in a fluidized bed with microwaves Abandoned US20060237300A1 (en)

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DE10260743.5 2002-12-23
DE10260743A DE10260743B4 (de) 2002-12-23 2002-12-23 Verfahren und Anlage zum thermischen Behandeln von körnigen Feststoffen in einem Wirbelbett
PCT/EP2003/013209 WO2004056468A1 (fr) 2002-12-23 2003-11-25 Traitement de solides granulaires dans un lit fluidise au moyen de micro-ondes

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US20080124253A1 (en) * 2004-08-31 2008-05-29 Achim Schmidt Fluidized-Bed Reactor For The Thermal Treatment Of Fluidizable Substances In A Microwave-Heated Fluidized Bed
US20090011118A1 (en) * 2006-02-03 2009-01-08 Glatt Gmbh Measurement, Monitoring and Control of Directed Product Movements in Fluidized Bed or Spouted Bed Systems and Suitable Systems
US7662351B2 (en) 2002-12-23 2010-02-16 Outotec Oyj Process and plant for producing metal oxide from metal compounds
US7854608B2 (en) 2002-12-23 2010-12-21 Outotec Oyj Method and apparatus for heat treatment in a fluidized bed
US7878156B2 (en) 2002-12-23 2011-02-01 Outotec Oyj Method and plant for the conveyance of fine-grained solids
US9370762B2 (en) 2011-11-11 2016-06-21 Microwave Chemical Co., Ltd. Chemical reaction apparatus
US9573112B2 (en) 2011-11-11 2017-02-21 Microwave Chemical Co., Ltd. Chemical reaction apparatus
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US10457930B2 (en) 2010-06-30 2019-10-29 Microwave Chemical Co., Ltd. Oil-based material-producing method and oil-based material-producing apparatus
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US8048380B2 (en) 2002-12-23 2011-11-01 Outotec Oyj Process and plant for producing metal oxide from metal compounds
US20060162500A1 (en) * 2002-12-23 2006-07-27 Dirk Nuber Fluidized bed method and plant for the heat treatment of solids containing titanium
US7651547B2 (en) 2002-12-23 2010-01-26 Outotec Oyj Fluidized bed method and plant for the heat treatment of solids containing titanium
US7662351B2 (en) 2002-12-23 2010-02-16 Outotec Oyj Process and plant for producing metal oxide from metal compounds
US20100074805A1 (en) * 2002-12-23 2010-03-25 Outotec Oyj Fluidized bed method for the heat treatment of solids containing titanium
US7854608B2 (en) 2002-12-23 2010-12-21 Outotec Oyj Method and apparatus for heat treatment in a fluidized bed
US7878156B2 (en) 2002-12-23 2011-02-01 Outotec Oyj Method and plant for the conveyance of fine-grained solids
US8021601B2 (en) 2002-12-23 2011-09-20 Outotec Oyj Plant for the heat treatment of solids containing titanium
US20080124253A1 (en) * 2004-08-31 2008-05-29 Achim Schmidt Fluidized-Bed Reactor For The Thermal Treatment Of Fluidizable Substances In A Microwave-Heated Fluidized Bed
US8187663B2 (en) * 2006-02-03 2012-05-29 Glatt Gmbh Measurement, monitoring and control of directed product movements in a Wurster-arrangement and suitable systems
US20090011118A1 (en) * 2006-02-03 2009-01-08 Glatt Gmbh Measurement, Monitoring and Control of Directed Product Movements in Fluidized Bed or Spouted Bed Systems and Suitable Systems
US10457930B2 (en) 2010-06-30 2019-10-29 Microwave Chemical Co., Ltd. Oil-based material-producing method and oil-based material-producing apparatus
KR101838330B1 (ko) 2011-06-29 2018-04-26 마이크로파 화학 주식회사 화학 반응 장치 및 화학 반응 방법
US11224852B2 (en) 2011-06-29 2022-01-18 Microwave Chemical Co., Ltd. Chemical reaction apparatus and chemical reaction method
US9370762B2 (en) 2011-11-11 2016-06-21 Microwave Chemical Co., Ltd. Chemical reaction apparatus
US9573112B2 (en) 2011-11-11 2017-02-21 Microwave Chemical Co., Ltd. Chemical reaction apparatus
US10464040B2 (en) 2011-11-11 2019-11-05 Microwave Chemical Co., Ltd. Chemical reaction method
US11229895B2 (en) 2011-11-11 2022-01-25 Microwave Chemical Co., Ltd. Chemical reaction method using chemical reaction apparatus
US20170203273A1 (en) * 2014-06-24 2017-07-20 Microwave Chemical Co., Ltd. Chemical reaction apparatus
US10744479B2 (en) * 2014-06-24 2020-08-18 Microwave Chemical Co., Ltd. Chemical reaction apparatus

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EA200501037A1 (ru) 2006-02-24
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NO20053289L (no) 2005-09-06
BR0317686A (pt) 2005-11-22
DE60305070D1 (de) 2006-06-08
ATE324940T1 (de) 2006-06-15
DE10260743A1 (de) 2004-07-08
NO20053289D0 (no) 2005-07-05
JP2006511775A (ja) 2006-04-06
WO2004056468A1 (fr) 2004-07-08
EP1575702A1 (fr) 2005-09-21
CA2510013A1 (fr) 2004-07-08
DE10260743B4 (de) 2008-05-15
PE20040454A1 (es) 2004-09-10
AU2003288160A1 (en) 2004-07-14
CN1729047A (zh) 2006-02-01

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