WO2024047295A1

WO2024047295A1 - Microwave calcination furnace for solid materials divided into fine particles

Info

Publication number: WO2024047295A1
Application number: PCT/FR2023/051118
Authority: WO
Inventors: Frédéric Vandenbussche
Original assignee: Innovation & Development Company
Priority date: 2022-08-29
Filing date: 2023-07-19
Publication date: 2024-03-07
Also published as: FR3139188A1

Abstract

The invention relates to a microwave calcination furnace for solid materials divided into fine particles, comprising a heating chamber of elongate form, a longitudinal axis of which is arranged vertically, an intake tube (8) opening into the heating chamber at an upper end of said heating chamber, a discharge port opening into the heating chamber at a lower end of said heating chamber, a mixer (28) comprising at least one mixing shaft (30) which carries a plurality of mixing blades (32) and a system (34) for rotating the mixing shaft, and at least one waveguide (18) which is connected to a microwave generator (20) and which opens into the heating chamber between the upper and lower ends of said heating chamber via a protection window (22) mounted on the heating chamber with interposed wave-cancelling seals (26).

Description

Title of the invention: Microwave calcination furnace for solid materials divided into fine particles

Technical area

[0001] The invention relates to the general field of microwave heating at high temperature to carry out calcination treatment (possibly continuously) of solid materials divided into fine particles, and in particular powders.

Prior art

[0002] Calcination heat treatment consists of heating an inert body to high temperature (with temperatures above 150°C and reaching 1900°C) in a closed enclosure in order to decompose it or obtain chemical reactions.

[0003] In the mining industry, calcination is used as a heat treatment process applied to ores such as kaolinite, clinker, bauxite, lithium and magnesite to obtain thermal decomposition, for example the elimination of l crystal clear water, CO2 removal or phase transformation of minerals.

[0004] During this treatment process, the bound metals (in ores or other solids) are converted into oxide (calcinate), in the form of powder, ash or dust, or undergo a phase transition by heating. The process is usually carried out in long cylindrical kilns or tall vertical burner kilns.

[0005] It is known to carry out such a process by calcining materials in powder form. We thus know the calcination of powders using rotary heating ovens with direct burner or by indirect heating of the oven wall. These calcination processes, however, present the disadvantages of being energy-intensive, emitters of significant quantities of CO2 and dust and with low efficiency.

We also know vertical “flash” ovens in which the powder to be treated is projected into a flame at high temperature for flash calcination. However, this calcination process is very energy-intensive and a source of a significant quantity of CO2 and dust that must be treated.

[0007] There are still vertical electric ovens with hot plates as described in publication CN 2656406. However, these ovens have low efficiency and are unsuitable for applications on an industrial scale.

[0008] We also know from publications FR 2,850,519 and FR 2,850,520 microwave radiation heating devices which process materials in batches (or batches) in a rotating cavity. These solutions have the advantages of allowing uniform heating, high temperature heat treatments and significant CO2 savings. On the other hand, applied to the treatment of powders, they can pose problems with the creation of electric arcs due to the flight of fines in the oven.

[0009] We also know from publication FR 2,965,907 a solution for heat treatment using continuous microwave radiation per turn. However, this technology is unsuitable for temperatures exceeding 600 to 700°C.

[0010] Publication CN 103822464 describes a process for heating kaolin type powders by microwaves in a multi-stage vertical oven. This oven has a series of cones made of microwave-heating material over which the product to be treated flows, which makes it possible to calcine products that do not react to microwaves. On the other hand, this type of oven has the disadvantages of creating dust and being poorly suited to industrial microwave heating (in particular due to a bed thickness which is low, damage and wear cones, and thermal runaways).

[0011] Publication CN102305541 describes a continuous process mixed with microwaves and traditional tower heating by gravity falling into a tube in which the The product is preheated by microwave then transferred to a rotating tube to finalize cooking. This process has the disadvantages of creating a large quantity of dust, which is a source of generation of electric arcs and which strongly limits microwave power.

[0012]We know from the publication WO 2009/034418 a microwave process making it possible to solve the problems linked to dust. This process consists of passing the product through a channel of rectangular section with an advance of the product generated by vibrations and distributing the waves over the top of this channel. Although effective, this process turns out to be completely unsuitable for use on an industrial scale and poses interface problems when the waves arrive and heating homogeneity.

Presentation of the invention

[0013] The present invention aims to respond to all of the aforementioned drawbacks by proposing a solution particularly suited to solid materials divided into fine particles such as powders and to implementation on an industrial scale.

[0014] In accordance with the invention, this goal is achieved thanks to a microwave calcination furnace for solid materials divided into fine particles, comprising:

- an elongated heating chamber with a longitudinal axis arranged vertically;

- at least one tube for admitting materials to be treated opening into the interior of the heating enclosure at an upper end thereof;

- at least one evacuation port for the treated materials opening inside the heating enclosure at a lower end thereof;

- a mixer mounted inside the heating enclosure and comprising at least one mixing shaft which is arranged parallel to the longitudinal axis of the heating enclosure and which carries a plurality of mixing blades, and a system for rotating the mixing shaft around its axis; And

- at least one wave guide which is connected to a microwave generator and which opens inside the heating enclosure between its upper and lower ends via a protective window mounted on the enclosure heating with interposition of wave trapping joints.

The oven according to the invention is remarkable in particular in that it allows the materials to be treated to be placed directly in contact with the microwave field, in their mass. The oven according to the invention makes it possible to circulate at a controlled speed the materials to be treated just in front of the arrival of the microwaves to heat them homogeneously, at a high power density while avoiding the creation of dust and optimizing the yield. In addition, the area subjected to microwaves is very limited because the waves are quickly damped in the product.

[0016] According to one embodiment, the heating chamber has a straight section of oblong shape with two half-cylinders.

[0017] In this embodiment, the mixer advantageously comprises two parallel mixing shafts, each centered on one of the axes of the two half-cylinders and each carrying a plurality of mixing blades, the mixing blades carried by the one of the mixing shafts interlocking with those carried by the other mixing shaft, which ensures optimal mixing.

[0018] Also preferably, the system for rotating the mixing shafts is configured to drive the two mixing shafts in opposite directions and at synchronized speeds, always with the aim of optimizing mixing.

[0019] More preferably, the protective window has a straight section of trapezoidal shape curved so as to fit the space not subject to the mixing blades carried by the two mixing shafts. [0020] According to an advantageous arrangement, the waveguide opens at a lower part of the heating enclosure so as to create a cold upper zone not subjected to microwaves and a hot lower zone subjected to microwaves. waves.

[0021] In this case, the heating enclosure is preferably provided at the cold zone with a thermal insulation coating.

[0022] Furthermore, the oven may further comprise induction heating means positioned above the waveguide so as to create an intermediate preheating zone located between the cold zone and the hot zone.

[0023] The oven may further comprise means for heating by Joule effect of the mixing blades located at least at the level of the preheating zone, which makes it possible to ensure additional heating of the materials to be treated.

[0024] According to an advantageous arrangement, the evacuation orifice of the treated materials opens inside the heating enclosure via a hopper and its flow rate is regulated by a valve with motorized adjustable opening .

[0025] According to another advantageous arrangement, the oven further comprises a plurality of temperature probes opening into the interior of the heating enclosure at different heights.

The heating enclosure may be provided with an external thermal insulation covering.

Preferably, each wave trapping joint comprises a plurality of grooves which extend over the entire periphery of the protective window and which have a depth equal to a quarter of the wavelength of the microwaves emitted.

[0028] According to an advantageous arrangement, the oven can comprise a plurality of wave guides positioned one above the other and connected to microwave generators delivering microwaves at different frequencies and powers in a different manner. to define several heating stages distributed over the height of the heating enclosure. Brief description of the drawings

[0029] [Fig. 1] Figure 1 is a schematic perspective view of a microwave calcination oven according to one embodiment of the invention.

[0030] [Fig. 2] Figure 2 is a front view of the oven of Figure 1.

[0031] [Fig. 3] Figure 3 is a side sectional view of the oven of Figure 1.

[0032] [Fig. 4] Figure 4 is a cross-section of the oven of Figure 1 in top view.

[0033] [Fig. 5] Figure 5 is a cross-sectional view showing a protective window according to one embodiment of the oven according to the invention.

[0034] [Fig. 6] Figure 6 is a front view of an oven according to a variant embodiment of the invention.

Description of embodiments

The invention relates to a thermal calcination treatment, which can be carried out continuously, of solid materials divided into fine particles, and in particular of powders. In the context of the present invention, the calcination heat treatment is carried out with heating temperatures of between 150°C and 1900°C.

[0036] Figures 1 to 5 represent, in different views, an oven 2 according to the invention intended for carrying out such a calcination heat treatment.

[0037] According to the invention, the oven 2 notably comprises a heating enclosure 4 of elongated shape and positioned so that its longitudinal axis X-X is substantially vertical.

[0038] In cross section (as shown in Figure 4), the heating chamber 4 of the oven according to the invention has an oblong shape, that is to say a shape elongated which is longer than wide and which ends in two half-cylinders each centered on a vertical axis Yl-Yl, Y2-Y2.

The heating chamber 4 is typically made of an electrically conductive material resistant to high temperatures, for example refractory steel. Its thickness is generally between 1 and 10mm and its dimensions include a length between 200mm and 5m and a width between 200mm and 2m.

The heating chamber 4 is also provided with an external thermal insulation covering (for example a layer of aluminized rock wool having a thickness of around 5mm - not shown in the figures).

[0041]At its upper end, the heating enclosure 4 is closed by an upper cover 6. At least one admission tube 8 of materials to be treated passing through this upper cover 6 opens into the interior of the enclosure heater 4 at an upper end thereof.

Likewise, at its lower end, the heating chamber 4 is closed by a bottom drain flange 10 in which a discharge orifice 12 for the treated materials is made.

[0043] Advantageously, this evacuation orifice 12 opens inside the heating enclosure via a hopper 14 and its flow rate is regulated by a valve with motorized adjustable opening 16.

[0044] Furthermore, the oven 2 according to the invention comprises at least one waveguide 18 which is connected to a microwave generator 20 and which opens into the interior of the heating enclosure 4 between its ends upper and lower.

Typically, the microwave generator 20 comprises a magnetron or klystron (having a unit power which can vary between 1kW and 10MW) coupled to a frequency generator (which can vary from 200MHz to 5000MHz).

[0046] In the example shown in Figures 1 to 6, two waveguides 18 are provided which are positioned vertically one above the other and which are each connected to a microwave generator different. GOOD Of course, the number of waveguides could be greater and distributed differently depending on the dimensions of the heating enclosure.

[0047] In the case of several waveguides positioned one above the other, the frequencies and powers of each microwave generator can be different in order to optimize the heating of the materials to be treated. In particular, it is particularly advantageous to have microwave generators with frequencies defined by heating stage for targeted materials. Likewise, it may be advantageous to be able to vary the power of each stage of microwave generators to optimize the heating efficiency of the materials.

[0048] Indeed, the response of a material to microwaves depends on its dielectric permittivity which varies as a function of the frequency of the electromagnetic field and the temperature of the product in the form of a function which is variable depending on the chemistry materials.

[0049] Preferably, the wave guide(s) 18 open(s) at a lower part of the heating enclosure 4 so as to create a cold upper zone ZF not subject to micro- waves and a hot lower zone ZC subjected to microwaves.

[0050] In this case, the heating chamber 4 is advantageously provided at the cold zone ZF with a thermal insulation covering 21 (Figure 3).

[0051]Each waveguide 18 opens into the interior of the heating enclosure 4 via a protective window 22 which is mounted in an opening of the heating enclosure by a mounting flange 24 with interposition of wave trapping joints 26.

[0052] The protective window 22 is made of a material transparent to microwaves generated by the wave generator and resistant to high temperatures. It is for example made of quartz or ceramic and makes it possible to isolate the waveguide from dust.

[0053] The interface between each protective window 22 and the heating enclosure 4 necessarily leaves retention zones. The disadvantage of these areas of retention is that they are immobile, so that heating them by microwaves causes thermal outbursts which can go as far as the vitrification of these zones and their damage.

[0054] Also, in order to cancel the effect of microwaves at these retention zones, it is planned to position wave trapping seals 26 all around each protection window. The effect of these wave trapping seals 26 is to cancel the effect of microwaves on the periphery of the protective window over a thickness of approximately 5mm corresponding to the retention zone between the protective window 22 and the heating chamber 4.

[0055] The principle of the wave trapping joints 26 is to cause part of the incident wave to travel an additional half-wavelength so that the other part of the wave is canceled at the same time. meeting.

[0056] As shown in particular in Figure 5, each wave trapping joint 26 thus comprises a plurality of grooves 26a which extend over the entire periphery of the protective window 22 and which have a depth P equal to a quarter of the wavelength of the microwaves emitted, such that one round trip corresponds to half a wavelength.

The geometry of these wave trapping joints 26 depends on the frequency of the microwaves emitted. For different magnetron frequencies, the dimensions of the wave trapping joints will therefore be different.

The oven 2 according to the invention also comprises a mixer 28 which is mounted inside the heating enclosure 4.

[0059] This mixer 28 comprises at least one mixing shaft 30 which is arranged parallel to the longitudinal axis X-X of the heating enclosure and which carries a plurality of mixing blades 32, as well as a drive system in rotation 34 of the mixing shaft around its axis.

The mixing shaft 30 extends from the upper end of the heating chamber 4 towards its lower end and the mixing blades 32 are regularly distributed over the entire height of the heating chamber. At the level from the upper end thereof, the mixing shaft 30 passes through the upper cover 6 and is connected to the rotational drive system 34.

[0061] In the exemplary embodiment of Figures 1 to 6, the mixer 28 comprises two mixing shafts 30a, 30b which are each centered on one of the axes Yl-Yl, Y2-Y2 of the two half-cylinders and which each carry a plurality of mixing blades 32a, 32b

[0062] In this configuration, the mixing blades carried by one of the two mixing shafts intertwine with those carried by the other mixing shaft so as to ensure optimal mixing of the materials to be treated (see Figure 4 notably).

[0063] Likewise, still in this configuration, the rotational drive system 34 of the mixing shafts 30a, 30b is advantageously configured to drive the two mixing shafts in opposite directions and at speeds synchronized with each other, always in the aim of improving the mixing of the materials to be treated.

[0064] For this purpose, as shown in particular in Figure 2, the rotational drive system 34 of the mixing shafts 30a, 30b consists for example of a geared motor assembly 34a which is connected to the mixing shafts by systems belts or gears 34b (figure 2). In addition, the mixing shafts are guided by bearings or bearings 36 (figure 3).

[0065] Furthermore, the mixing blades 32a, 32b are dimensioned so that the mixing of the materials to be treated is carried out over the entire height of the heating chamber and to give the material a fluid behavior.

[0066] Preferably, the shafts 30a, 30b and mixing blades 32a, 32b are coated with an insulating ceramic allowing operation at high temperatures (up to approximately 1900°C) and avoiding excessive wear.

[0067] Also preferably, as shown in Figure 5, each protective window 22 has a straight section of trapezoidal shape curved so as to fit the space not subject to the mixing blades 32a, 32b carried by the two mixing shafts 30a, 30b. The operation of the oven 2 according to the invention is as follows.

[0069] The materials to be treated which are introduced into the heating chamber 4 through the inlet tube(s) 8 are brought in a continuous and fluid layer by the rotation of the mixing blades 32a, 32b in front of the outlets of the wave guides 18 to be heated uniformly in their volume.

[0070] It will be noted that the ratio between the diameter of the intake tube(s) 8 and their length makes it possible, for a given frequency of the microwave generator 20, to cancel wave leaks (for example 60 mm in diameter and 100mm in length for a microwave generator frequency of 2450MHz).

[0071] The materials to be treated are immediately mixed by the mixing blades 32a, 32b and penetrate regularly into a cold zone ZF not subject to microwaves, adding to the mass of product already present in the enclosure heating.

[0072] When the product reaches the heating zone ZC, the microwaves emitted by the waveguides 18 penetrate a layer of 1 to 10 cm or more of product depending on the frequency of the microwave generator 20 ( approximately 2 to 5cm for a frequency of 2450MHz and 5 to 20cm for a frequency of 915MHz) and the type of material to be processed. The rotation of the mixing blades 32a, 32b ensures that all particles pass in front of the protective windows 22.

[0073] The product descends as it is calcined to the low point of the heating chamber where it is recovered by the hopper 14 and then collected by the evacuation port 12.

[0074] It will be noted that the heating temperatures are measured by temperature probes 38 opening into the interior of the heating enclosure 4 at different heights thereof.

[0075] It will also be noted that the control of the heating, the flow of products and the power emission of the different microwave generators can be carried out by a automaton and a man-machine interface. [0076] In connection with Figure 6, we will now describe an alternative embodiment of the oven according to the invention.

[0077] In this variant embodiment, the oven 2' further comprises induction heating means 40 which are positioned above the waveguide(s) 18 so as to create an intermediate preheating zone ZPC located between the cold zone ZF and the hot zone ZC.

[0078] This variant makes it possible to heat the heating chamber 4 in the preheating zone ZPC in order to preheat the product to be treated.

[0079] According to another variant of the oven not shown in the figures, the mixing shafts and the mixing blades that they carry can be heated by the Joule effect over a certain height, preferably corresponding to the ZPC preheating zone described above .

[0080]This variant is particularly suitable up to temperatures of around 600/700°C by allowing additional heating of the product to be treated.

Claims

[Claim 1] Calcination furnace (2; 2') by microwave for solid materials divided into fine particles, comprising:

- a heating chamber (4) of elongated shape, a longitudinal axis (X-X) of which is arranged vertically;

- at least one intake tube (8) of materials to be treated opening into the interior of the heating enclosure at an upper end thereof;

- at least one evacuation port (12) for the treated materials opening inside the heating enclosure at a lower end thereof;

- a mixer (28) mounted inside the heating enclosure and comprising at least one mixing shaft (30) which is arranged parallel to the longitudinal axis of the heating enclosure and which carries a plurality of blades mixing (32), and a drive system (34) in rotation of the mixing shaft around its axis; And

- at least one waveguide (18) which is connected to a microwave generator (20) and which opens inside the heating enclosure between its upper and lower ends via a protective window (22) mounted on the heating enclosure with the interposition of wave trapping joints (26), in which:

- the heating chamber (4) has a straight section of oblong shape with two half-cylinders, and

- the mixer comprises two parallel mixing shafts (30a, 30b), each centered on one of the axes (Yl-Yl, Y2-Y2) of the two half-cylinders and each carrying a plurality of mixing blades (32a, 32b ), the mixing blades carried by one of the mixing shafts intertwining with those carried by the other mixing shaft.

[Claim 2] Oven according to claim 1, in which the drive system (34a, 34b) in rotation of the mixing shafts (30a, 30b) is configured to drive the two mixing shafts in opposite directions and at synchronized speeds .

[Claim 3] Oven according to one of claims 1 and 2, in which the protective window (22) has a straight section of trapezoidal shape curved so as to fit the space not subject to the mounted mixing blades (32a, 32b ) by the two mixing shafts.

[Claim 4] Oven according to any one of claims 1 to 3, in which the waveguide (18) opens at a lower part of the heating enclosure so as to create an upper cold zone (ZF ) not subjected to microwaves and a lower hot zone (ZC) subjected to microwaves.

[Claim 5] Oven according to claim 4, in which the heating enclosure (') is provided at the cold zone (ZF) with a thermal insulation covering (21).

[Claim 6] Furnace according to one of claims 4 and 5, further comprising induction heating means (40) positioned above the waveguide (18) so as to create an intermediate preheating zone (ZPC ) located between the cold zone (ZF) and the hot zone (ZC).

[Claim 7] Oven according to claim 6, further comprising means for heating by Joule effect of the mixing blades located at least at the level of the preheating zone (ZPC).

[Claim 8] Oven according to any one of claims 1 to 7, in which the evacuation orifice (12) of the treated materials opens inside the heating enclosure (4) via of a hopper (14) and its flow rate is regulated by a motorized adjustable opening valve (16).

[Claim 9] Oven according to any one of claims 1 to 8, further comprising a plurality of temperature probes (38) opening into the interior of the heating enclosure at different heights.

[Claim 10] Oven according to any one of claims 1 to 9, in which the heating enclosure (4) is provided with an external thermal insulation covering.

[Claim 11] Furnace according to any one of claims 1 to 10, wherein each wave trapping joint (26) has a plurality of grooves (26a) which extend over the entire periphery of the window. protection (22) and which have a depth (P) equal to a quarter of the wavelength of the microwaves emitted.

[Claim 12] Oven according to any one of claims 1 to 11, comprising a plurality of waveguides (18) positioned one above the other and connected to microwave generators (20) delivering micro -waves at different frequencies and powers so as to define several heating stages distributed over the height of the heating enclosure (4).