AU2003288152A1 - Method and plant for the thermal treatment of granular solids in a fluidized bed - Google Patents
Method and plant for the thermal treatment of granular solids in a fluidized bed Download PDFInfo
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- AU2003288152A1 AU2003288152A1 AU2003288152A AU2003288152A AU2003288152A1 AU 2003288152 A1 AU2003288152 A1 AU 2003288152A1 AU 2003288152 A AU2003288152 A AU 2003288152A AU 2003288152 A AU2003288152 A AU 2003288152A AU 2003288152 A1 AU2003288152 A1 AU 2003288152A1
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- fluidized
- wave guide
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- fluidized bed
- bed reactor
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- 239000007787 solid Substances 0.000 title claims description 73
- 238000000034 method Methods 0.000 title claims description 44
- 238000007669 thermal treatment Methods 0.000 title claims description 13
- 239000007789 gas Substances 0.000 claims description 95
- 230000005855 radiation Effects 0.000 claims description 19
- 238000005243 fluidization Methods 0.000 claims description 14
- 238000005192 partition Methods 0.000 claims description 11
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 238000001354 calcination Methods 0.000 description 6
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- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 6
- 229910052737 gold Inorganic materials 0.000 description 6
- 239000010931 gold Substances 0.000 description 6
- 230000003647 oxidation Effects 0.000 description 6
- 238000007254 oxidation reaction Methods 0.000 description 6
- 239000011028 pyrite Substances 0.000 description 6
- NIFIFKQPDTWWGU-UHFFFAOYSA-N pyrite Chemical compound [Fe+2].[S-][S-] NIFIFKQPDTWWGU-UHFFFAOYSA-N 0.000 description 6
- 229910052683 pyrite Inorganic materials 0.000 description 6
- 238000002485 combustion reaction Methods 0.000 description 5
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- 230000009467 reduction Effects 0.000 description 4
- 238000012546 transfer Methods 0.000 description 4
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 229910052717 sulfur Inorganic materials 0.000 description 3
- 239000011593 sulfur Substances 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 229910052964 arsenopyrite Inorganic materials 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
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- 230000005672 electromagnetic field Effects 0.000 description 2
- 239000011019 hematite Substances 0.000 description 2
- 229910052595 hematite Inorganic materials 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- LIKBJVNGSGBSGK-UHFFFAOYSA-N iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Fe+3].[Fe+3] LIKBJVNGSGBSGK-UHFFFAOYSA-N 0.000 description 2
- 230000010355 oscillation Effects 0.000 description 2
- 239000002918 waste heat Substances 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910005432 FeSx Inorganic materials 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- XUHJGXBPMAPKDW-UHFFFAOYSA-N [As].[Fe]=S Chemical compound [As].[Fe]=S XUHJGXBPMAPKDW-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- MJLGNAGLHAQFHV-UHFFFAOYSA-N arsenopyrite Chemical compound [S-2].[Fe+3].[As-] MJLGNAGLHAQFHV-UHFFFAOYSA-N 0.000 description 1
- 230000001174 ascending effect Effects 0.000 description 1
- 238000009529 body temperature measurement Methods 0.000 description 1
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- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000006735 deficit Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
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- 239000000446 fuel Substances 0.000 description 1
- 238000004868 gas analysis Methods 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
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- 238000011144 upstream manufacturing Methods 0.000 description 1
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Classifications
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- 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
-
- 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
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- 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
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- 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
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- 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
-
- 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
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- 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
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- 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
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00245—Avoiding undesirable reactions or side-effects
- B01J2219/00247—Fouling of the reactor or the process equipment
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Combustion & Propulsion (AREA)
- Metallurgy (AREA)
- Mechanical Engineering (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Geology (AREA)
- Electromagnetism (AREA)
- Toxicology (AREA)
- Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
- Crucibles And Fluidized-Bed Furnaces (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Description
WO 2004/056471 PCT/EP2003/013162 METHOD AND PLANT FOR THE THERMAL TREATMENT OF GRANULAR SOLIDS IN A FLUIDIZED BED 5 Technical Field 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 10 corresponding plant. 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 15 guide occluded with a microwave-transparent substance (window). The type of decoupling the microwaves from the feed conduit can be effected in different ways. Theoretically, 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 20 circuit comprising coil and capacitor towards very high frequencies. Theoretically, such oscillating circuit can likewise be operated free of loss. In the case of a substantial increase of the resonance frequency, 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 25 wave guide cross-section. In reality, 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 30 oscillating circuit thereto, which withdraws energy from the first one. Similarly, by flanging a second wave guide to a first wave guide energy can be decoupled from the same (wave guide transition). When the first wave guide is shut off behind the coupling point by a shorting plunger, the entire energy can even be diverted to the second wave guide.
WO 2004/056471 PCT/EP2003/013162 -2 The microwave energy in a wave guide is enclosed by the electrically conductive walls. In the 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. 5 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 10 end. When 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. When the field lines of the wall currents in wave guides are interrupted by slots, 15 microwave energy emerges from the wave guide through these slots (slot decoupling), as the energy cannot flow on in the wall. The wall currents in a rectangular wave guide flow parallel to the center line on the middle of the broad side of the wave guide, and transverse to the center line on the middle of the narrow side of the wave guide. Transverse slots in the broad side and longitudinal slots in the narrow side therefore 20 decouple microwave radiation from wave guides. 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 25 mathematics, as the Maxwell equations (unsteady, nonlinear differential equations) must ultimately be solved with the corresponding marginal conditions. In the case of a rectangular or round wave guide cross-section, however, 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, 30 and due to the relatively easy producibility, 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. These standard dimensions were adopted in Germany, which is why odd dimensions appear in part. In general, all industrial microwave sources of the WO 2004/056471 PCT/EP2003/013162 -3 frequency 2.45 GHz are equipped with a rectangular wave guide of the typ R26, which has a cross-section of 43 x 86 mm. In wave guides, different oscillation states exist: In the transversal electric mode (TE mode), the electric field component lies transverse to the wave guide direction and the magnetic component lies in wave guide direction. In 5 the transversal magnetic mode (TM mode), the magnetic field component lies transverse to the wave guide direction and the electric component lies in wave guide direction. Both oscillation states can appear in all directions in space with different mode numbers (e.g. TE-1-1, TM-2-0). 10 A method for the thermal treatment of granular solids is known from US 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 . There is employed a stationary 15 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. 20 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. Open wave guides involve the risk that the microwave source is soiled by dust and gases and damaged in the course of time. This can be avoided by microwave-transparent windows, which occlude 25 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. Description of the Invention 30 It is therefore the object underlying the invention to make the feeding of microwaves into a stationary or circulating fluidized bed more efficient and protect the microwave source against resulting gases, vapors and/or dusts.
WO 2004/056471 PCT/EP2003/013162 -4 In accordance with the invention, this object is substantially solved in a method as mentioned above in that a gas stream is fed into the fluidized-bed reactor through the wave guide, which is also used for introducing microwaves. Thus, the microwave source is disposed outside the stationary or circulating fluidized bed, the microwave 5 radiation being fed into the fluidized-bed reactor through at least one wave guide and a gas stream being passed through the wave guide in addition to the microwave radiation. By means of the gas stream from the wave guide it is reliably avoided that dust or process gases enter the wave guide, spread up to the microwave source and damage the same. In accordance with the invention, microwave-transparent windows in 10 the wave guide for shielding the microwave source, as they are commonly used in the prior art, 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. 15 An improvement of the method is achieved when the gas stream introduced through the wave guide contains gases which react with the fluidized bed and in the case of a circulating fluidized-bed reactor can even be utilized for an additional fluidization of the fluidized bed. Thus, part of the gas which so far has been introduced into the fluidized 20 bed through other supply conduits is used for dedusting the wave guide. As a result, providing neutral purge gas can also be omitted. Another improvement is obtained in accordance with the invention when the gas stream introduced through the wave guide has a temperature difference with respect to the 25 gases and solids present in the fluidized-bed reactor. In this way, additional heat can specifically be introduced into the fluidized bed or the fluidized bed can be cooled, depending on the desired effect. The thermal treatment can not only be effected in a stationary, but also in a circulating 30 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. Usually, the amount of solids circulating per hour is at least three times the amount of solids present in the fluidized-bed reactor.
WO 2004/056471 PCT/EP2003/013162 -5 The solids can also be passed through at least two succeeding fluidized-bed reactors, for instance two fluidization chambers separated from each other by means of weirs or partitions, in which the stationary fluidized beds are formed and to which the 5 electromagnetic waves (microwaves) coming from wave guides are fed. The solids can move from one fluidized-bed reactor into the adjacent fluidized-bed reactor. One variant consists in that between the two adjacent fluidized-bed reactors an intermediate chamber is disposed, which is in particular connected with both fluidization chambers and contains a fluidized bed of granular solids, the intermediate chamber having no 10 associated wave guide. Another variant of the method of the invention consists in that a partition with the opening in the bottom region is used for separating the two fluidization chambers. To a particular advantage, the operating conditions, in particular temperature, 15 composition of the fluidizing gas, energy input and/or fluidization rate can be specified differently for each of several fluidized-bed reactors. In the case of one fluidized bed or several succeeding fluidized beds, the solids thus can for instance first be passed through a preheating chamber upstream of the first fluidized bed. Furthermore, downstream of the last fluidized bed serving the thermal treatment a cooling chamber 20 may be provided for cooling the solid product. Another advantage is obtained in that solid deposits in the wave guide are avoided by the continuous gas stream through the wave guide. These solid deposits change the cross-section of the wave guide in an undesired way and absorb part of the microwave 25 energy which was designed for the solids in the fluidized bed. Due to the absorption of energy in the wave guide, the same is heated very much, whereby the material is subject to a strong thermal wear. In addition, solid deposits in the wave guide effect undesired feedbacks to the microwave source. 30 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. Preferably, the ISM frequencies 435 MHz, 915 MHz and 2.45 GHz are used.
WO 2004/056471 PCT/EP2003/013162 Expediently, the optimum frequencies are determined for each application in a trial operation. In accordance with the invention, the wave guide wholly or largely consists of 5 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 adapted to the frequency used. 10 The temperatures in the fluidized bed lie for instance in the range from 300 to 12000C, and it may be recommended to introduce additional heat into the fluidized bed, e.g. through indirect heat transfer. For temperature measurement in the fluidized bed, insulated sensing elements, radiation pyrometers or fiber-optic sensors can be used. 15 In accordance with the invention, 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. The Particle-Froude-Numbers are defined as follows: u Frp U_ * Fy E*dpg 20 with u = effective velocity of the gas flow in m/s Ps = density of the solid particles or process gases penetrating into the wave guide in kg/m 25 pf = effective density of the purge gas in kg/m 3 dp = mean diameter in m of the particles of the reactor inventory (or the particles formed) during operation of the reactor g = gravitational constant in m/s 2 . 30 To prevent solid particles or generated process gases from the reactor from penetrating into the wave guide, gas serving as purge gas flows through the wave guide. Solid WO 2004/056471 PCT/EP2003/013162 -7 particles can for instance be dust particles present in the reactor or also the treated solids. Process gases are generated in the processes which take place in the reactor. By specifying certain Particle-Froude-Numbers, the density ratio of the penetrating solid particles or process gases to the purge gas is considered in accordance with the 5 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 penetrating particles. Substances can thereby be prevented from penetrating into the wave guide. For most applications, a Particle-Froude-Number between 2 and 30 is preferred. 10 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 15 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 SO2. 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 20 by the thermal treatment can easily be disposed of. Expediently, 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 25 temperatures. The present invention furthermore relates to a plant in particular for performing the above-described method for the thermal treatment of granular solids in a fluidized bed. A plant in accordance with the invention includes a fluidized-bed reactor, a microwave 30 source disposed outside the fluidized-bed reactor, and a wave guide for feeding the microwave radiation into the fluidized-bed reactor, a gas supply conduit for feeding gas into the fluidized-bed reactor being connected to the wave guide.
WO 2004/056471 PCT/EP2003/013162 -8 Furthermore, the reactor can be elongated and have a gas-permeable bottom for the entrance of fluidizing gas, for instance a bottom provided with hole or slot openings, bell nozzles or similar openings suitable for fluidization technology. This reactor designed as fluidized-bed channel can be installed horizontally or with a small angle of 5 inclination of a few degrees and have a length/width ratio of at least 1.5 to 1, for instance 4 to 1. In such a reactor, the treatment and the transport of the granular solids can easily be realized in accordance with the invention. To divide the fluidization channel reactor in several zones, partitions or weirs can be arranged inside the fluidized bed formed in the channel and/or in the gas space located above the fluidized 10 bed, depending on the process, an opening being left for the passage of the granular solids. It is particularly advantageous when the partitions or weirs are adjustable for separating zones, so that the height of the fluidizing material and the slot height can be varied for the transfer from zone to zone. The bed depth in the fluidization channel is selected such that in each zone an almost uniform energy state is achieved due to a 15 thorough mixing. In the case of a suitable fluidizing material, the siphon principle can also be used instead of transfer weirs. Microwave inlet openings with wave guides connected thereto can be provided in all zones or in individual zones. Developments, advantages and possibilities for applying the present invention can also 20 be taken from the following description of examples and from the drawing. All described and/or illustrated features per se or in any combination belong to the subject-matter of the invention, independent of their inclusion in the claims or their back-reference. Brief Description of the Drawings 25 In the drawings Fig. 1 shows the thermal treatment of granular solids in a stationary fluidized bed in a schematic representation; 30 Fig. 2 shows a method variant with a circulating fluidized bed; and Figs. 3, 4, 5, 6 show method variants with a plurality of stationary fluidized beds.
WO 2004/056471 PCT/EP2003/013162 -9 Detailed Description of the Preferred Embodiments 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 5 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. In a chamber, the solids form a stationary fluidized bed 3 which is traversed by a fluidizing gas, e.g. air. For this purpose, the fluidizing gas is 10 passed from below through a gas distributor 4 into the fluidized bed 3. In the upper region of the fluidized-bed reactor 1, an open wave guide 5, which leads to a microwave source 7, is connected to the chamber with the stationary fluidized bed 3. 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 15 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 into the fluidized-bed reactor 1 and prevents the ingress of dust or process gases from the chamber with the fluidized bed 3 into the wave guide 5. In this way, the microwave source 7 is protected against being damaged, and at the same 20 time microwave-absorbing soil deposits in the wave guide 5 are prevented without the open wave guide 5 having to be closed by a window transparent for microwaves. If necessary for the process, 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 25 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. In Fig. 2, the fluidized-bed reactor 1 constitutes a reactor with a circulating fluidized bed 30 (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 conduit 11 and introduced into a solids separator 12. The solids separated therein are at least partly WO 2004/056471 PCT/EP2003/013162 -10 recirculated through a return conduit 13 into the lower region of the circulating fluidized layer 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 a discharge conduit 5 15. The fluidizing gas for forming the circulating fluidized bed, e.g. air, is supplied to the fluidized-bed reactor 1 through a conduit 4a and then first gets into a distribution chamber 4h, before it flows into the fluidized-bed reactor 1 through a grid 4i, entrains the introduced, in particular fine-grained solids and forms a circulating fluidized layer as fluidized bed. 10 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. In addition, purge gas from conduit 6 flows through the wave guide 5, in order to avoid the ingress 15 of dirt as well as deposits in the wave guide 5. In the present case as well, the inner region of the chamber can again be provided with one or more heat exchangers for additionally heating the granular solids, which for a better clarity was not represented in Fig. 2. 20 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. 25 As shown in Fig. 3, two stationary fluidized-bed reactors 1 and la are arranged in series, an intermediate chamber 1c being located between the chambers of the two reactors 1 and la. In all three chambers, the solids form a stationary fluidized bed 3, 3a, which is traversed by fluidizing gas. The fluidizing gas for each chamber is supplied through a separate conduit 4a, 4b, 4c, respectively. The granular solids to be treated 30 enter the first fluidized-bed reactor 1 through conduit 2, and completely treated solids leave the second fluidized-bed reactor la through the discharge conduit 10. From the upper region of the chamber of the first reactor 1 a first wall 19 extends downwards. However, it does 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 WO 2004/056471 PCT/EP2003/013162 -11 fluidized bed 3a of the intermediate chamber 1c. The intermediate chamber 1c extends up to a weir-like second wall 21, over which the solids from the fluidized bed 3a of the intermediate chamber 1c are moved into the chamber of the second fluidized-bed reactor la. Corresponding to the plants as shown in Figs. 1 and 2, wave guides 5 with 5 purge air conduits 6 and microwave sources 7 are each connected to the chambers of the two reactors 1 and la, through which wave guides the microwaves and purge gas are fed into the reactors 1 and la. In the chambers of the reactors 1 and la, heat exchanging elements 8 may be arranged in addition. 10 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 la and the intermediate chamber 1c, by the vertical wall 19. For the gas spaces 22, 23 separate gas discharge conduits 9 and 9a exist. As a result, different conditions can be maintained in the chambers of the reactors 1 and la, in particular different 15 temperatures can exist or different fluidizing gases can be supplied through separate gas supply conduits 4a, 4b, 4c. Furthermore, 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. 20 As shown in Fig. 4, two stationary fluidized-bed reactors 1 and la without intermediate chamber are arranged directly succeeding each other, a partition 19 being disposed between the two. In the chambers of the two reactors 1, la the solids form a stationary fluidized bed 3, 3a, which is fluidized by fluidizing gas from several conduits 4a, 4b, 4c 25 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 la through the discharge conduit 10. From the upper region of the chamber of the first reactor 1, 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 30 which solids from the first fluidized bed 3 can get into the fluidized bed 3a of the second fluidized-bed reactor la. Waveguides 5, which are connected to the microwave sources 7, each extend to the two chambers of the reactors 1 and l a. According to the principle described already in the previous embodiments, microwaves are fed into the two reactors 1, la through these open wave guides 5, in order to heat the solids to be WO 2004/056471 PCT/EP2003/013162 -12 treated, which absorb the microwave radiation, and reach the necessary process temperatures. At the same time, purge gas flows into the wave guides 5 through purge air conduits 6, in order to avoid deposits in the same. In the chambers of the reactors 1 and la, heat exchanging elements 8 may be arranged in addition. 5 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 la, by the vertical wall 19. There exist separate gas discharge conduits 9 and 9a. As a result, different conditions can be maintained in the different reactor chambers 1 and 10 la; in particular, the temperatures or the gas phase composition can be different. Different fluidizing gases can also be supplied through the respective conduits 4a, 4b, 4c. Furthermore, the two microwave sources 7 can be designed differently and perform different functions. 15 In the arrangement as shown in Fig. 5, the solids to be treated, which are supplied via conduit 2, first enter an antechamber 31 and flow through a first intermediate chamber 32 in the first fluidized-bed reactor 1. The solids then are discharged from the same to flow through a second intermediate chamber Ic into the second fluidized-bed reactor la and finally through the third intermediate chamber 33 into a cooling chamber 34, 20 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 la, in order to feed microwaves into the reactors 1 and la according to the above-described principle. All chambers include stationary fluidized beds, to which fluidizing gas is supplied through separate gas 25 supply conduits 4a to 4g for each chamber. The exhaust gases are discharged through corresponding conduits 9a to 9d. In the cooling chamber 34, the fluidized bed includes a cooling means 35 for an indirect heat transfer, whose cooling fluid, e.g. cooling water, is heated in the cooling means 35 30 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.
WO 2004/056471 PCT/EP2003/013162 -13 As variant of another plant in accordance with the invention, Fig. 6 shows a fluidization channel reactor 38, in which the fluidized layer is formed in a channel-type bottom 39 with through openings for a fluidizing gas. The fluidization channel reactor 38 is divided into four zones 41a to 41d separated by adjustable partitions 40, the first zone 41a 5 constituting a preheating zone, the second zone 41b an oxidation zone, the third zone 41c a reduction zone, and the fourth zone 41d a cooling zone. Downstream of each of the zones 41a to 41d a separator 42 or a cyclone is provided, which separates the solids discharged with the fluidizing gas from the gas stream and recirculates the same to the respective zone 41a to 41d. To achieve a high utilization of energy, the exhaust 10 gases from the separators 42 are supplied to other zones 41a to 41d by means of a suitable gas recirculation. Via a feed conduit 43, the solids to be treated are supplied to the first zone 41a of the reactor 38. As fluidizing gas, hot exhaust gas from a first combustion chamber 44 is 15 supplied to the first zone 41a, in order to dry and preheat the introduced material. The correspondingly preheated solids flow through the partition 40 into the oxidation zone 41b, to which there is likewise supplied hot exhaust gas from a second combustion chamber 45. To both combustion chambers 44, 45, supply conduits are connected for fuel and air and possibly preheated exhaust gas from other process zones 41a to 41d. 20 From the oxidation zone 41b, the solids are supplied to the reduction zone 41c. For protecting the downstream compressor, the exhaust gas from the oxidation zone 41b can likewise be supplied to the reduction zone 41c via a cooler 47. Possibly, the exhaust gas is again heated in a heater 49. 25 To bring the fluidized material to the desired energy state, microwave rays are additionally introduced into the oxidation zone 41a and the reduction zone 41c through wave guides 46 traversed by purge gas. Due to the microwave radiation, the solids are heated by an internal excitation, so that the energy state can easily be adjusted. In the last zone 41d, the treated material is cooled with injected air and discharged as product 30 through the discharge conduit 48. To make the feeding of microwaves into a stationary or circulating fluidized bed 3, 3a more efficient and also protect the microwave source 7 against the resulting gases, vapors and dusts, the microwave source 7 in accordance with the invention is disposed WO 2004/056471 PCT/EP2003/013162 -14 outside the stationary or circulating fluidized bed 3, 3a and the fluidized-bed reactors 1, la, 38. The microwave radiation is fed into the fluidized-bed reactor 1, la, 38 through at least one open wave guide 5, 46, wherein in addition to the microwave radiation a gas stream flows into the fluidized-bed reactor 1, la, 38 through the wave guide 5, 46. 5 By means of the gas stream, the wave guide 5, 46 is kept dust-free, which considerably increases the efficiency of the introduction of microwaves. Example 1 (Calcination of ores containing pyrite) 10 Pyrite with grain sizes in the range from 80 to 160 pm is treated in two successive fluidized beds 3, 3a, which are designed corresponding to the plant in accordance with Fig. 4. Irradiation is effected in both chambers by microwaves with a frequency of 2.45 GHz. As radiation source, magnetrons are used. 15 Into the first fluidized-bed reactor 1, 182.5 kg/h pyrite are charged. For fluidizing the fluidized bed 3, 360 Nm3/h nitrogen are used, which are supplied through conduit 4a, so that a height of 20 cm is obtained for the fluidized bed. After the microwave treatment, the mass flow rate of the solid reaction products from the first fluidized-bed reactor 1 is 20 153.5 kg/h. The first chamber is operated at 5500C and a magnetron irradiation of 36 kW. Deoiled compressed air with a volume flow rate of 120 Nm 3 /h is supplied to the second fluidized bed 3a through conduit 4c. The second chamber is operated at 5000C and a 25 microwave irradiation of 36 kW. After 90 min, a steady state is obtained; after the microwave treatment, the mass flow rate of the solid reaction products is 140.2 kg/h. As purge gas, there is each utilized the gas used for fluidization, i.e. in the first chamber nitrogen and in the second chamber deoiled compressed air, which each have 30 a volume flow rate of 50 Nm3/h. The phase content of the pyrite used and of the products of the first and second process stages is analysed by X-ray diffraction. In the pyrite, only FeS 2 can be detected. After the first temperature treatment, the solids consist of substoichiometric WO 2004/056471 PCT/EP2003/013162 -15 FeS and FeS 2 for instance in accordance with FeSx with x = 1.4. After the second stage, no more sulfur-containing products can be detected, the solids virtually exclusively consist of hematite. 5 Example 2 (Calcination of ore containing gold) On a laboratory scale, gold ore with grain sizes in the range below 250 pm is treated in a circulating fluidized bed which is designed as shown in Fig. 2. Irradiation is effected by microwaves with a frequency of 2.45 GHz. As radiation source, a magnetron is 10 used. For purging, 24 Nm 3 /h air are supplied to the reactor 1 through the wave guide 5. Feed Type gold ore, ground, dried and classified Grain fraction 15 Max pm 250 Composition Wt-% Org. C 1.05 CaCO 3 19.3 20 A1 2 0 3 12.44 FeS 2 2.75 Inerts, e.g. SiC 2 64.46 Input, about kg 100 25 Apparatus Type of reactor circulating fluidized bed with microwave irradiation Reactor diameter mm 200 Magnetron 500 W, 2.45 GHz Microwave coupling wave guide, R26 (43 x 86 mm) designed as secondary air conduit 30 Connected: online gas analysis + exhaust gas washing Operation: continuous WO 2004/056471 PCT/EP2003/013162 -16 Test conditions and results Inlet Outlet Mass flow rate, gold ore feed kg/h 195 Primary air 0C 250 5 Nm 3 /h 30 0C 50 Oil consumption kg/h 0.70 Secondary air, preheated by means of Luvo to 0C 425 10 Secondary air, consumption Nm 3 /h 24 Drier air 0C 50 320 Nm 3 /h 70 70 Calcining residue, ex-WS luvo 0C 400 kg/h 182 15 Calcining gas, total Nm 3 /h 59 0C 600 Composition, dry 20 CO2 vol-% 23.3
N
2 vol-% 74.3 02 vol-% 2.4
SO
2 ppV 134.1 25 The phase content of the material used and of the products is analysed by X-ray diffraction. After the treatment, neither residual sulfur nor organic carbon can be detected in the calcining residue, the solids have a pale gray color.
WO 2004/056471 PCT/EP2003/013162 -17 List of Reference Numerals: 1,1a fluidized-bed reactor 20 opening Ic intermediate chamber 21 weir, partition 5 2 conduit 31 antechamber 3,3a fluidized layer, fluidized bed 32 intermediate chamber 4 gas distributor 33 intermediate chamber 4a to gconduits 34 cooling chamber 4h distribution chamber 35 cooling means 10 4i grid 36 conduit 5 wave guide 37 heat exchanger 6 conduit 38 fluidization channel reactor 7 microwave source 39 bottom 8 heat exchanger 40 partitions 15 9 conduit, gas discharge conduit 41a to d zones 10 discharge conduit 42 separator 11 conduit 43 feed conduit 12 solids separator 44 combustion chamber 13 return conduit 45 combustion chamber 20 14 discharge conduit 46 wave guide 15 discharge conduit 47 cooler 16 waste heat boiler 48 discharge conduit 17 dedusting 49 heater 19 weir, partition 25
Claims (13)
1. A method for the thermal treatment of granular solids in a fluidized bed (3, 3a) which is located in a fluidized-bed reactor (1, la, 38), wherein microwave radiation is 5 fed into the fluidized-bed reactor (1, la, 38) through at least one wave guide (5, 46), characterized in that a gas stream is fed into the fluidized-bed reactor (1, la, 38) through the same wave guide (5, 46).
2. The method as claimed in claim 1, characterized in that the gas stream 10 introduced through the wave guide (5, 46) contains gases which react with the fluidized bed (3, 3a).
3. The method as claimed in claim 1 or 2, characterized in that the gas stream introduced through the wave guide (5, 46) is additionally utilized for a fluidization of the 15 fluidized bed (3, 3a).
4. The method as claimed in any of the preceding claims, characterized in that heat is additionally supplied to the fluidized bed (3, 3a) through the introduced gas stream. 20
5. The method as claimed in any of claims 1 to 3, characterized in that the fluidized bed (3, 3a) is cooled by the introduced gas stream.
6. The method as claimed in any of the preceding claims, characterized in that 25 the fluidized bed (3, 3a) is part of a stationary and/or circulating fluidized bed.
7. The method as claimed in any of the preceding claims, characterized in that the reactor comprises at least two fluidized-bed reactors (1, la, 41a to d), which are separated from each other by weirs or partitions (19, 21, 40) such that solids can move 30 as moving bed from one fluidized-bed reactor (1, 41a to c) into an adjacent fluidized bed reactor (la, 41b to d).
8. The method as claimed in claim 7, characterized in that the operating conditions, in particular temperature, composition of the fluidizing gas, energy input WO 2004/056471 PCT/EP2003/013162 -19 and/or fluidization rate, can be specified differently for each fluidized-bed reactor (1, la, 41a to d).
9. The method as claimed in any of the preceding claims, characterized in that by means of the gas stream introduced into the wave guide (5, 46) solid deposits in the 5 wave guide (5, 46) are avoided.
10. The method as claimed in any of the preceding claims, characterized in that the used frequency of the microwave radiation lies between 300 MHz and 30 GHz, preferably at the frequencies 435 MHz, 915 MHz and 2.45 GHz. 10
11. The method as claimed in any of the preceding claims, characterized in that the temperatures in the fluidized bed (3, 3a) lie between 3000C and 12000C.
12. The method as claimed in any of the preceding claims, characterized in that 15 the Particle-Froude-Number Frp in the wave guide (5, 46) is 0.1 to 100, preferably 2 to
30. 13. A plant for the thermal treatment of granular solids in a fluidized bed (3, 3a), in particular for performing the method as claimed in any of claims 1 to 12, comprising a 20 fluidized-bed reactor (1, la, 38), a microwave source (7) disposed outside the fluidized bed reactor (1, la, 38) and a wave guide (5, 46) for feeding the microwave radiation into the fluidized-bed reactor (1), characterized in that a gas supply conduit (6) is connected to the wave guide (5, 46) for feeding gas into the fluidized-bed reactor (1, l a, 38). 25 14. The plant as claimed in claim 13, characterized in that the wave guide (5) has a rectangular or round cross-section, whose dimensions are adapted in particular to the used frequency of the microwave radiation. 30 15. The plant as claimed in claim 13 or 14, characterized in that the wave guide (5, 46) has a length of 0.1 m to 10 m.
Applications Claiming Priority (3)
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DE10260742A DE10260742A1 (en) | 2002-12-23 | 2002-12-23 | Process and plant for the thermal treatment of granular solids in a fluidized bed |
DE10260742.7 | 2002-12-23 | ||
PCT/EP2003/013162 WO2004056471A1 (en) | 2002-12-23 | 2003-11-24 | Method and plant for the thermal treatment of granular solids in a fluidized bed |
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AU2003288152A1 true AU2003288152A1 (en) | 2004-07-14 |
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AU2003288152A Abandoned AU2003288152A1 (en) | 2002-12-23 | 2003-11-24 | Method and plant for the thermal treatment of granular solids in a fluidized bed |
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EP (1) | EP1587614A1 (en) |
JP (1) | JP2006512554A (en) |
CN (1) | CN1729049A (en) |
AU (1) | AU2003288152A1 (en) |
BR (1) | BR0317683A (en) |
CA (1) | CA2510792A1 (en) |
DE (1) | DE10260742A1 (en) |
EA (1) | EA200501035A1 (en) |
NO (1) | NO20053265L (en) |
PE (1) | PE20040448A1 (en) |
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JP2008173521A (en) * | 2006-08-09 | 2008-07-31 | Honda Electronic Co Ltd | Submerged plasma treatment apparatus and submerged plasma treatment method |
CN102268559A (en) | 2007-05-21 | 2011-12-07 | 奥贝特勘探Vspa有限公司 | Processes for extracting aluminum and iron from aluminous ores |
JP5603134B2 (en) * | 2010-05-13 | 2014-10-08 | マイクロ波化学株式会社 | Chemical reaction apparatus and chemical reaction method |
JP4874411B2 (en) * | 2010-05-13 | 2012-02-15 | マイクロ波環境化学株式会社 | Chemical reaction apparatus and chemical reaction method |
JP5901519B2 (en) | 2010-06-30 | 2016-04-13 | マイクロ波化学株式会社 | Oily substance manufacturing method and oily substance manufacturing apparatus |
AU2012231686B2 (en) | 2011-03-18 | 2015-08-27 | Aem Technologies Inc. | Processes for recovering rare earth elements from aluminum-bearing materials |
US9410227B2 (en) | 2011-05-04 | 2016-08-09 | Orbite Technologies Inc. | Processes for recovering rare earth elements from various ores |
WO2012162817A1 (en) | 2011-06-03 | 2012-12-06 | Orbite Aluminae Inc. | Methods for preparing hematite |
US11224852B2 (en) | 2011-06-29 | 2022-01-18 | Microwave Chemical Co., Ltd. | Chemical reaction apparatus and chemical reaction method |
WO2013037054A1 (en) | 2011-09-16 | 2013-03-21 | Orbite Aluminae Inc. | Processes for preparing alumina and various other products |
US11229895B2 (en) | 2011-11-11 | 2022-01-25 | Microwave Chemical Co., Ltd. | Chemical reaction method using chemical reaction apparatus |
JP5109004B1 (en) | 2011-11-11 | 2012-12-26 | マイクロ波化学株式会社 | Chemical reactor |
JP5114616B1 (en) * | 2011-11-11 | 2013-01-09 | マイクロ波化学株式会社 | Chemical reactor |
RU2016104423A (en) | 2012-01-10 | 2018-11-22 | Орбит Текнолоджис Инк. | METHODS FOR PROCESSING RED SLUR |
CA2862307C (en) | 2012-03-29 | 2015-12-01 | Orbite Aluminae Inc. | Processes for treating fly ashes |
BR112015000626A2 (en) | 2012-07-12 | 2017-06-27 | Orbite Aluminae Inc | processes for preparing titanium oxide and other miscellaneous products |
US9353425B2 (en) | 2012-09-26 | 2016-05-31 | Orbite Technologies Inc. | Processes for preparing alumina and magnesium chloride by HCl leaching of various materials |
CA2891427C (en) | 2012-11-14 | 2016-09-20 | Orbite Aluminae Inc. | Methods for purifying aluminium ions |
JP5763234B1 (en) * | 2014-02-27 | 2015-08-12 | マイクロ波化学株式会社 | Chemical reactor |
JP5702016B1 (en) | 2014-06-24 | 2015-04-15 | マイクロ波化学株式会社 | Chemical reactor |
JP5997816B2 (en) * | 2015-07-14 | 2016-09-28 | マイクロ波化学株式会社 | Chemical reaction apparatus and chemical reaction method |
DE102016103100A1 (en) * | 2016-02-23 | 2017-08-24 | Outotec (Finland) Oy | Process and apparatus for the thermal treatment of granular solids |
CN107899519B (en) * | 2017-11-02 | 2020-09-29 | 中石化炼化工程(集团)股份有限公司 | System for Fischer-Tropsch synthesis and method for preparing low-carbon olefin from synthesis gas |
GB2570501A (en) * | 2018-01-29 | 2019-07-31 | Mortimer Tech Holdings Limited | Process for treating a material |
CN110396594B (en) * | 2019-08-21 | 2021-06-08 | 东北大学 | Microwave continuous suspension roasting method for enhancing iron and phosphorus increase and reduction of high-phosphorus oolitic hematite |
FR3136541A1 (en) * | 2022-06-14 | 2023-12-15 | Innovation & Development Company | microwave and fluidized bed calcination furnace |
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US3528179A (en) * | 1968-10-28 | 1970-09-15 | Cryodry Corp | Microwave fluidized bed dryer |
GB1560545A (en) * | 1975-07-31 | 1980-02-06 | Buehler Ag Geb | Method for drying pasta prducts and apparatus for bulk material tretment |
JPS5745335A (en) * | 1980-09-02 | 1982-03-15 | Mitsui Eng & Shipbuild Co Ltd | Heating fluidized bed reactor |
FR2750348B1 (en) * | 1996-06-28 | 1998-08-21 | Conte | PROCESS FOR INCREASING THE WET RESISTANCE OF A BODY, BODY THUS PROCESSED AND ITS APPLICATIONS |
WO1998008989A1 (en) * | 1996-08-27 | 1998-03-05 | Emr Microwave Technology Corporation | Method for microwave induced oxidation of sulphidic ore material in fluidized bed without sulphur dioxide emissions |
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2002
- 2002-12-23 DE DE10260742A patent/DE10260742A1/en not_active Withdrawn
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- 2003-11-24 AU AU2003288152A patent/AU2003288152A1/en not_active Abandoned
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- 2003-11-24 CN CNA2003801073090A patent/CN1729049A/en active Pending
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BR0317683A (en) | 2005-11-29 |
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NO20053265D0 (en) | 2005-07-04 |
DE10260742A1 (en) | 2004-07-08 |
PE20040448A1 (en) | 2004-09-10 |
NO20053265L (en) | 2005-09-06 |
WO2004056471A1 (en) | 2004-07-08 |
JP2006512554A (en) | 2006-04-13 |
CA2510792A1 (en) | 2004-07-08 |
ZA200505911B (en) | 2006-11-29 |
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