The present technology is directed to apparatus, systems and methods for calcining minerals.
Calcination typically involves heating a feedstock (e.g., a mineral) in the presence of a processing fluid (e.g., air or oxygen) in an apparatus (referred to herein as a “calciner”) to cause thermal decomposition, phase transition, or devolatization. The reaction vessel may feature various shapes and designs depending on the mineral, required temperature, processing fluid, and many other factors. Some designs, for example open tube and pot calciners, disadvantageously permit particles and/or processing fluids to escape before the reaction occurs due to flow dynamics, resulting in lost material, inefficiencies and increased costs. Improved calciners and methods of calcination are needed.
In some embodiments, the present technology provides a calciner comprising a crucible, a heating element in proximity to the crucible and configured to heat the contents of the crucible, and optionally a delivery tube configured to provide a processing fluid to the crucible and/or to be articulated in a pattern within the crucible.
In other embodiments, the present technology provides a calciner comprising a crucible, a heating element in proximity to the crucible and configured to heat the contents of the crucible, a dome configured to seal a first portion of the crucible to enable a positive pressure to be applied to the first portion of the crucible, a conduit positioned through the dome configured to enable the positive pressure to be applied through the conduit to the first portion of the crucible, an insulated tube positioned through the dome and having a first end positioned in the first portion of the crucible, and a dispensing port configured to selectively enable material to be dispensed from the first portion of the crucible.
In other embodiments, the present technology provides a crucible assembly comprising an outer shell, an inner crucible housed inside the outer shell, a loading assembly disposed at least partially within the inner crucible and configured to enable material to be loaded or unloaded from the inner crucible, and may include a load-spreading insulating layer disposed between the outer shell and the inner crucible, the load-spreading insulating layer and may comprise a first heating element, and/or a second heating element, and/or at least one high strength filament.
In some embodiments, the present technology provides a method of preparing a calcined powder, the method comprising loading a precursor material into a calciner, heating the precursor material in the presence of a processing fluid, agitating the precursor material during at least a portion of the step of heating to form a calcined powder and/or and agglomerated form of such powder, and/or extracting the calcined powder and/or portions of the agglomerated form of the powder from the calciner.
These and other embodiments are described in more detail below.
Various examples of apparatus, systems and methods for calcining and processing feedstock substances will now be described in further detail. The following description provides specific details for a thorough understanding and enabling description of these examples. One skilled in the relevant art will understand, however, that the techniques discussed herein may be practiced without many of these details. Likewise, one skilled in the relevant art will also understand that the technology can include many other features not described in detail herein. Additionally, some well-known steps, structures or functions may not be shown or described in detail below so as to avoid unnecessarily obscuring the relevant description.
The terminology used below is to be interpreted in its broadest reasonable manner, even though it is being used in conjunction with a detailed description of some specific examples of the embodiments. Indeed, some terms may even be emphasized below; however, any terminology intended to be interpreted in any restricted manner will be overtly and specifically defined as such in this section.
In some embodiments, the present technology provides a calciner. The calciner comprises a component such as a tube or a crucible generally configured to enable a feedstock to be inserted therein, and is in proximity (e.g., is adjacent to or includes) one or more heating elements configured to transfer heat to the feedstock.
Referring now to
The feedstock 104 may comprise, consist of, or consist essentially of any suitable feedstock for calcining (e.g., to produce a calcined product such as a catalyst, a glass, a glass ceramic, and/or a ceramic). For example, the feedstock 104 may comprise one or more of: a metal, a mineral, and/or a recycled product that requires removal of water, carbon dioxide, volatile materials, and/or other unwanted substances. In some embodiments the feedstock 104 includes mineral concentrate, scrap iron, aluminum, magnesium, nickel, molybdenum, etc., various carbonates such as calcium, magnesium and/or potassium carbonates, along with other oxides such as silica, alumina, and/or calcium oxide. In some embodiments, the feedstock 104 is selected from the group consisting of: a hydroxide such as aluminum hydroxide, magnesium hydroxide, and/or calcium hydroxide, and/or a compound containing a rare earth substance.
The crucible 102 may be constructed of any suitable material that permits energy transmission such as radiation or heat transfer to the intended feedstock 104, yet is resistant to the temperatures and reactivity of the intended feedstock 104. For example, the crucible 102 may be formed of a refractory ceramic material such as alumina, magnesia, spinel, quartz, or fused silica; or a refractory metal selection including alloys from the platinum family. In some embodiments, the crucible 102 is formed of a composited ceramic material. The size and shape of the crucible 102 are not particularly limited; in some embodiments the crucible 102 has a cup or pot shape, such as a cylinder or tapered cylinder.
The one or more heating elements 106 can be located in close proximity to the crucible 102 in order to maximize efficiency of heat transfer to the feedstock 104 (e.g., through the wall(s) of the crucible 102). In some embodiments, the heating elements 106 are inductive heating elements and/or resistive elements which are operably connected to a controllable energy source.
The delivery tube 108 is oriented such that a distal end is within the crucible 102 while the proximal end is external to the crucible 102. The delivery tube 108 is configured to enable a processing fluid to be introduced to the crucible 102, and may be formed of any suitable material that is resistant to the temperature of the calcination process and to the reactivity of the feedstock and processing fluids. The processing fluid may include air, nitrogen, hydrogen, argon, oxygen, a halogen, and/or a nitrogen donor such as ammonia. In some embodiments, the delivery tube 108 may additionally configured to be articulated in a pattern 110, for example to sweep any suitable pattern 110 within the feedstock 104.
Referring now to
As shown in
The processing reactant may be any suitable processing reactant including, but not limited to a halogen (e.g., bromine, iodine, chlorine and/or fluorine), oxygen, nitrogen, hydrogen, a transition metal carbonyl, a silane, and/or other fluids that provide metal or semiconductor donor capabilities. In embodiments wherein the processing reactant is a halogen, the electrolyzer 302 may be configured to convert a corresponding aqueous halogen salt or a corresponding fused halogen salt into its atomic components (e.g., a halogen processing reactant and a byproduct) via electrolytic decomposition. In some embodiments, other process reactants such as oxygen and/or hydrogen may be collected through manifold 304 and delivered through the second flexible conduit 322 and the second pressure regulator 316 to storage tank 318.
Calciners 100, 200 and 300 can be operated in batch or semi-continuous operations. In batch operations, feedstock 104 is added to the crucible 102 and after the desired conversion in some applications the calcined product may be melted and cast, extruded, or drawn from the crucible 102 for further processing. In semi-continuous operations, new feedstock 104 can be continuously or intermittently added to the crucible 102. In addition or in the alternative, calcined product produced by the calcination process can be removed from the crucible 102 as powder, prill or any other suitable agglomerated form.
In some embodiments, the calciner is configured to be operated continuously. One such embodiment is shown in
Calciner 400 includes a crucible 102 configured to hold a feedstock 104, at least one heating element 106 and a delivery tube 108 each configured substantially similar to that described with respect to
In some embodiments, the calciner 400 includes a dispensing port 450 configured to enable melted material 406 to be removed from the crucible 102 under positive pressure and/or by force of gravity. The dispensing port 450 may include bell lips 426 to form a seal with the inner surface of the crucible 102, for example under positive pressure applied through the delivery tube 108. In some embodiments, the dispensing port 450 includes bottom check valve 416. The dispensing port may be heated (e.g., by heating elements 418 and/or 420). In some embodiments, the bottom check valve 416 is activated by operation of a solenoid 418. The extracted calcined product 424 may have a cross-sectional shape similar to that of the shape of the dispensing port 450, such as in the shape of a tube, a bar, a strip etc.
In some embodiments, a process gas may be introduced through conduit 410 and/or through the dispensing port 450. For example, in some embodiments, the process gas is produced by an electrolyzer similar to electrolyzer 302 shown in
As shown in
High strength filaments 512 and/or axial reinforcing filaments 514 are disposed between the first and second insulating layers 504A, 504B in a suitable pattern (e.g., a lattice) to increase the strength and/or rigidity (e.g., hoop strength) of the calciner 500. The high strength filaments 512 and the axial reinforcing filaments 514 may comprise any suitable material including, for example, carbon filaments, silicon carbide, glass-ceramics, selected metals, and/or ceramic fibers.
An outer shell 502 surrounds the outermost insulating layer 504A or 504B and provides electrical, thermal, chemical and mechanical protection and support of the calciner components. The outer shell 502 may be formed of a refractory ceramic material such as alumina, magnesia, spinel, quartz, or fused silica; or a refractory metal including alloys from the platinum family.
In operation, assembly 518 provides loading of material to be pre-melt processed including calcining, removal of water including water of hydration, de-aeration, and mixing of precursor ingredients that are subsequently conveyed from zone 520 and added to melt zone 522. Heating elements 106 and/or 508 provide heat production in melt zone 522 to enable final melting and refinement including chemical process and temperature adjustments required to extrude, draw, gob and press mold parts made of the composition dispensed from zone 522.
Any calciner of the present technology may further include additional features and elements common to calciners known in the art. For example, any calciner provided herein may further include instrumentation (e.g., sensors) configured to monitor and control the temperature, pressure, and other conditions of operation of each zone and respective process. The calciners of the present disclosure may be operatively connected to a controller (e.g., a computer) configured to control one or more operating parameters (e.g., temperature, time of heating, flow rate of the processing fluid and/or the process reactant, etc.).
As shown in
The step 610 of loading the precursor material into the calciner may comprise providing a feedstock and loading the feedstock into the calciner 100, 200, 300, 400 or 500 (e.g., into the crucible 102). In some embodiments, the step 610 is performed as a batch process. In such embodiments, a bolus of feedstock is loaded into the calciner and the step 630 of heating the precursor material begins after the bolus of feedstock is loaded into the calciner. In other embodiments, the step 610 of loading the precursor material is performed continuously. In such embodiments, the feedstock is continuously or semicontinuously loaded into the calciner 100, 200, 300, 400 or 500 (e.g., into the crucible 102) while at least a portion of the step 630 of heating the precursor material is also performed.
In step 620, a processing fluid is introduced into the calciner 100, 200, 300, 400 or 500 (e.g., into the crucible 102). The processing fluid may be introduced through a delivery tube 108 or a conduit 410 as described more fully above. In some embodiments, the step 620 of introducing the processing fluid comprises generating the processing fluid, for example by electrolysis of a substrate.
In step 630, heat is applied to the precursor material through the walls of the crucible 102. The may be accomplished by energizing the heating elements (e.g., inductive and/or resistive heating elements 106, 508). The heat may be applied to the feedstock for a predetermined time, or may be applied until a phase transition or other endpoint parameter is detected by a sensor. In embodiments wherein the calcination method is continuous, the heat may be applied for a predetermined time by transporting the feedstock through the crucible at a predetermined rate corresponding to a desired residence time (e.g., a desired mean or median residence time). Step 630 may further comprise agitating the precursor material, for example by articulating a pattern 110 with a delivery tube 108 in order to sweep a similar pattern to pattern 110 within the feedstock 104.
In some embodiments, the step 620 of introducing the processing fluid and/or the step 630 of heating the precursor material comprises applying positive pressure to the crucible 102. In some embodiments, the positive pressurization is provided by introducing a surplus of the processing fluid in step 620. In addition or in the alternative, the positive pressurization may be provided by heating the crucible 102 in step 630 after sealing the crucible 102 with a removable cover 102, 202. After step 630, at least a portion of the feedstock (e.g., some of the feedstock, most of the feedstock, substantially all of the feedstock, or all of the feedstock) has been calcined.
The step 640 of extracting the calcined powder may comprise any suitable method of removing the calcined powder from the crucible. In some embodiments, the calcined powder is removed in a melt form, for example through a dispensing port 450 or through a through an insulated tube 414. In some embodiments, the extracted melted calcined powder is cooled and optionally ground to form the calcined powder
Heating by resistive and/or inductive elements such as 106 along with process gas treatments enables very rapid processing of inexpensive feedstocks, such as minerals and recycled materials, glass, ceramic, and metals such as aluminum, magnesium, steel, stainless steel and super alloys. Final temperature adjustments with inductive and/or resistive elements 420 and/or 418 provides precision performance of finishing operations such as various heat treating and/or nucleation processes along with extrusion, drawing, and/or gob-molding in compression forming tooling.
In some embodiments, the method 600 further includes heat treating the dispensed material 412 and/or 424, for example by surface quenching, to retain amorphous surface layers that are compressively loaded by balancing tensile loading of subsurface zones that are characterized various degrees and orientations of crystallized microstructures. In some embodiments, the method 600 includes reheating and/or controlled cooling for various purposes, case hardening, or other modifications by introduction of one or more nucleating and/or compounding agents such as boron, nitrogen, oxygen, fluorine, carbon, silicon, and/or other substances.
Embodiments of the methods disclosed herein provide calcination of feedstock substances to form powders and/or agglomerated forms. Such powders and agglomerated forms may be used for any application in which calcined powders produced by other means are typically used.
While this specification contains many specifics, these should not be construed as limitations on the scope of any invention or of what may be claimed, but rather as descriptions of features that may be specific to particular embodiments of particular inventions. Certain features that are described in this specification in the context of separate embodiments can also be implemented in combination in a single embodiment. Conversely, various features that are described in the context of a single embodiment can also be implemented in multiple embodiments separately or in any suitable subcombination. Moreover, although features may be described above as acting in certain combinations and even initially claimed as such, one or more features from a claimed combination can in some cases be excised from the combination, and the claimed combination may be directed to a subcombination or variation of a subcombination.
Similarly, while operations are depicted in the drawings in a particular order, this should not be understood as requiring that such operations be performed in the particular order shown or in sequential order, or that all illustrated operations be performed, to achieve desirable results. In certain circumstances, multitasking and parallel processing may be advantageous. Moreover, the separation of various system components in the embodiments described above should not be understood as requiring such separation in all embodiments.
Only a few implementations and examples are described and other implementations, enhancements and variations can be made based on what is described and illustrated in this application.
From the foregoing, it will be appreciated that specific embodiments of the invention have been described herein for purposes of illustration, but that various modifications may be made without deviating from the scope of the invention. Accordingly, the invention is not limited except as by the appended claims.
This application claims priority to U.S. provisional patent application Ser. No. 61/863,832, filed on Aug. 8, 2013, the entire contents of which are incorporated herein by reference and relied upon.
Filing Document | Filing Date | Country | Kind |
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PCT/US14/50431 | 8/8/2014 | WO | 00 |
Number | Date | Country | |
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61863832 | Aug 2013 | US |