Molten Metal Reactors and Processes
20250171866 ยท 2025-05-29
Assignee
Inventors
Cpc classification
International classification
Abstract
A molten metal reactor comprising at least the following components a) through c): a) a reactor vessel comprising a molten metal bath, b) an injection assembly, and c) a product removal assembly.
Claims
1. A molten metal reactor comprising at least the following components a) through c): a) a reactor vessel comprising a molten metal bath, b) an injection assembly, and c) a product removal assembly.
2. The molten metal reactor of claim 1, wherein the reactor further comprises a partition located within the reactor vessel.
3. The molten metal reactor of claim 1, wherein the reactor further comprises 1 plug unit(s).
4. The molten metal reactor of claim 3, wherein each plug unit is used to seal in a positive pressure, inert gas purge, to reduce the amount of oxygen that can leak into the reactor.
5. The molten metal reactor of claim 3, wherein each plug unit is removable.
6. The molten metal reactor of claim 3, wherein the bottom surface of each plug unit is inserted into the molten metal bath.
7. The molten metal reactor of claim 3, wherein each plug unit is over an open surface of the reactor vessel when the reactor is in operation.
8. The molten metal reactor of claim 1 wherein the injection assembly is located on a plug unit.
9. The molten metal reactor of claim 1, wherein the injection assembly comprises 1 injection device(s).
10. The molten metal reactor of claim 9, wherein at least one injection device is used to inject at least one carbon source into the molten metal bath.
11. The molten metal reactor of claim 10, wherein the at least one carbon source is at least one hydrocarbon.
12. The molten metal reactor of claim 9, wherein at least one injection device is used to inject at least one inert gas into the molten metal bath.
13. The molten metal reactor of claim 12, wherein the at least one inert gas is argon.
14. The molten metal reactor of claim 9, wherein a portion of each injection device is inserted beneath the surface of the molten metal bath, at an angle relative to the base surface of a plug unit.
15. The molten metal reactor of claim 14, wherein the angle is from 35 degrees to 60 degrees, relative to the base surface of the plug unit.
16. The molten metal reactor of claim 1, wherein the molten metal of the molten metal bath comprises aluminum (Al), magnesium (Mg), lithium (Li), or any combination thereof.
17. The molten metal reactor of claim 1, wherein the molten metal of the molten metal bath comprises aluminum (Al), magnesium (Mg) or any combination thereof.
18. The molten metal reactor of claim 1, wherein the molten metal of the molten metal bath comprises aluminum (Al).
19. The molten metal reactor of claim 1, wherein the reactor comprises a closed-circuit recirculating system.
20. The molten metal reactor of claim 1, wherein the reactor further comprises from 1 to 25 electric resistance heaters.
21. The molten metal reactor of claim 20, wherein the heating element of each heater is inserted vertically into the molten bath.
22. The molten metal reactor of claim 20, wherein the electrical power generated by each heater is dissipated as heat into the molten metal bath.
Description
BRIEF DESCRIPTION OF THE DRAWINGS
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DETAILED DESCRIPTION
[0031] As discussed above, a molten metal reactor is provided, comprising at least the following components a) through c): a) a reactor vessel comprising a molten metal bath; b) an injection assembly; and c) a product removal assembly.
[0032] A molten metal reactor may comprise a combination of two or more embodiments as described herein. A molten metal process may comprise a combination of two or more embodiments as described herein.
[0033] The claims at the end of this application set out features of the reactors and/or processes described herein. The various advantages of such features will be better understood by reference to the following description of illustrative embodiments, read in conjunction with the figures introduced above. The following embodiments apply to both the reactors and processes, unless otherwise noted.
[0034] In one embodiment, or a combination of two or more embodiments, each described herein, a molten metal process takes place using the molten metal reactor 1 as shown in
[0035] The carbon particles and gas(es) flow into the collection chamber E, and are then transferred to two cyclone separators G (or 14), arranged in a parallel configuration. Each cyclone separator G is used to separate the particulate carbon from the gas stream (containing one or more gases). This is done typically through a vortex separation and/or a centripetal force. The remaining material and gas(es) then flow into a cyclone separator G, in a series configuration with the first two separators. In each cyclone separator G, the particulate matter drops into a collection drum (or barrel) H (or 16). The gases (predominantly argon) and the remaining carbon particles flow toward a recirculation fan in the axial position J (or 18), through the recirculating piping L (or 22). Additional particulate matter is collected in each drop tube K (or 20), and the argon is circulated back to the collection chamber E. Gases other than the inert gas, may be separated via a vent in in the collection chamber, and may be collected using one or more other devices. As shown in
[0036] It is noted, that to initially form the molten metal bath, metal ingots (for example, aluminum ingots) are added to the reactor vessel. The ingots are melted using one or more gas burners installed on one or more removable plug units. Examples of gas burners include natural gas forced air burners. Once the temperature of the bath is established at a temperature of about 80 degrees Fahrenheit higher than the operational bath temperature (ingots are in liquid form), as noted by several thermocouples placed inside the bath, the heating system for the reactor is carefully and controllably transferred from a phase 1gas burner system, to an intermediate phase 2gas burner/electric resistance heater system, and then carefully and controllably transferred from this phase 2 system, to a phase 3electric resistance heater system. Each gas burner is removed and replaced with an electric resistance heater. This process is continued until all the gas burners are replaced with electric resistance heaters. An electric resistance heater 30 is shown in
[0037] In one embodiment, or a combination of two or more embodiments, each described herein, referring to
[0038] In one embodiment, or a combination of two or more embodiments, each described herein, a product removal assemble configuration 68 is shown in
[0039] In one embodiment, or a combination of two or more embodiments, each described herein, referring to
[0040] In one embodiment, or a combination of two or more embodiments, each described herein, as shown in
[0041] In one embodiment, or a combination of two or more embodiments, each described herein, a cross-sectional view of the operation of a slag rake assembly 80 during a reaction is shown in
[0042] With any molten metal bath, the exposure of the bath surface to the atmosphere results a continuous absorption of oxygen and the formation of slag. This reduces the efficiency of the molten bath and results in the depletion of the bath, due to the formation of the slag. In one embodiment, or a combination of two or more embodiments, each described herein, the amount of exposure to oxygen is reduced by using a series of plug units. See
[0043] A removable plug unit 130, on which a circulation pump 140 is mounted, is shown in
[0044] In one embodiment, or a combination of two or more embodiments, each described herein, a launder makeup vessel 150, as shown in
[0045] In one embodiment, or a combination of two or more embodiments, each described herein, an injection assembly 64, mounted to a plug unit 130, is shown in
[0046] In one embodiment, or a combination of two or more embodiments, each described herein, the reactor further comprises a partition located within the reactor vessel.
[0047] In one embodiment, or a combination of two or more embodiments, each described herein, the reactor further comprises 1 plug unit(s), or 2 plug units. In one embodiment, or a combination of two or more embodiments, each described herein, each plug unit is used to seal in a positive pressure, inert gas purge, to reduce the amount of oxygen that can leak into the reactor. In one embodiment, or a combination of two or more embodiments, each described herein, each plug unit is removable. In one embodiment, or a combination of two or more embodiments, each described herein, the bottom surface of each plug unit is inserted into the molten metal bath. In one embodiment, or a combination of two or more embodiments, each described herein, one or more plug units are placed over the open surfaces of the reactor vessel when the reactor is in operation. In one embodiment, or a combination of two or more embodiments, each described herein, each plug unit may provide structural support for one or more other pieces of equipment.
[0048] In one embodiment, or a combination of two or more embodiments, each described herein, the injection assembly is located on a plug unit. In one embodiment, or a combination of two or more embodiments, each described herein, the injection assembly comprises 1 injection device(s), or 2 injection devices.
[0049] In one embodiment, or a combination of two or more embodiments, each described herein, at least one injection device is used to inject at least one carbon source into the molten metal bath. In one embodiment, or a combination of two or more embodiments, each described herein, the at least one carbon source is at least one hydrocarbon. In one embodiment, or a combination of two or more embodiments, each described herein, the at least one hydrocarbon is acetylene or methane, and further acetylene.
[0050] In one embodiment, or a combination of two or more embodiments, each described herein, at least one injection device is used to inject at least one inert gas into the molten metal bath. In one embodiment, or a combination of two or more embodiments, each described herein, the at least one inert gas is argon. The inert gas, such as argon, may be used to reduce the surface tension of the metal atoms and/or metal ions on the surface of the molten metal. The inert gas, such as argon, may be used to help degas the molten metal bath, such as an aluminum bath, to release trapped gas(es), such as hydrogen, from the bath.
[0051] In one embodiment, or a combination of two or more embodiments, each described herein, a portion of each injection device is inserted beneath the surface of the molten metal bath, at an angle relative to the base surface of a plug unit. In one embodiment, or a combination of two or more embodiments, each described herein, the angle is 35 degrees, or 40 degrees, or 45 degrees and/or 60 degrees, or 55 degrees, or 50 degrees, relative to the base surface of the plug unit.
[0052] In one embodiment, or a combination of two or more embodiments, each described herein, the ratio of the volume of the inert gas injected into the molten metal bath (V.sub.IG) to the volume of the carbon source injected into the molten metal bath (V.sub.CS), or V.sub.IG/V.sub.CS, is 0.70, or 0.75, or 0.80, or 0.85, or 0.90, or 0.95, or 1.00 and/or 1.40, or 1.35, or 1.30, or 1.20, or 1.15, or 1.10, or 1.05.
[0053] In one embodiment, or a combination of two or more embodiments, each described herein, the molten metal of the molten metal bath comprises aluminum (Al), magnesium (Mg), lithium (Li), or any combination thereof. In one embodiment, or a combination of two or more embodiments, each described herein, the molten metal of the molten metal bath comprises aluminum (Al), magnesium (Mg) or any combination thereof.
[0054] In one embodiment, or a combination of two or more embodiments, each described herein, the molten metal of the molten metal bath comprises aluminum (Al). In one embodiment, or a combination of two or more embodiments, each described herein, the aluminum (Al) is present in an amount 80 wt %, or 85 wt %, or 90 wt %, or 92 wt %, or 94 wt %, or 96 wt %, 98 wt %, or 99 wt %, based on the weight of the molten metal bath and/or present in an amount 100 wt %, based on the weight of the molten metal bath.
[0055] In one embodiment, or a combination of two or more embodiments, each described herein, the reactor comprises a closed-circuit recirculating system.
[0056] In one embodiment, or a combination of two or more embodiments, each described herein, each physical piece of equipment, used in the reactor, and which comes into contact with the molten metal, is independently coated with a refractory material. In one embodiment, or a combination of two or more embodiments, each described herein, the refractory material comprises boron nitride.
[0057] In one embodiment, or a combination of two or more embodiments, each described herein, the reactor further comprises 1 electric resistance heater, or 2 electric resistance heaters, or 3 electric resistance heaters, or 4 electric resistance heaters, or 5 electric resistance heaters, or 6 electric resistance heaters, or 7 electric resistance heaters, or 8 electric resistance heaters. In one embodiment, or a combination of two or more embodiments, each described herein, the reactor further comprises 25 electric resistance heaters, or 20 electric resistance heaters, or 15 electric resistance heaters, or 10 electric resistance heaters. In one embodiment, or a combination of two or more embodiments, each described herein, the heating element of each heater is inserted vertically into the molten bath. In one embodiment, or a combination of two or more embodiments, each described herein, the electrical power generated by each heater is dissipated as heat into the molten metal bath. This helps to reduce the dissipation of heat (energy) away from the molten metal bath.
DEFINITIONS
[0058] The term molten metal process, as used herein, refers to a process to carry out one or more chemical reactions by use of a molten metal bath, and, optionally, to separate and/or collect the one or more reaction products. The molten metal bath may be a molten metal alloy bath.
[0059] The term molten metal reactor, as used herein, refers to an assembly of devices used to carry out one or more chemical reactions using a molten metal bath, and, optionally, to separate and/or collect the one or more reaction products.
[0060] The term reactor vessel, as used herein, refers to a container that contains a molten metal bath. A molten metal bath comprises one or more metals. The reactor vessel is typically a refractory structure.
[0061] The term molten metal bath, as used herein, refers to a mass comprising one or more metals in a molten state, and where the bath is contained in a container, such as, for example, a crucible or other refractory container, or a refractory lined reactor vessel. The molten metal may comprise aluminum (Al), magnesium (Mg), lithium (Li), or any combination thereof.
[0062] The term carbon source, as used herein, refers to a chemical compound comprising one or more carbon atoms
[0063] The term hydrocarbon, as used herein, refers to a chemical compound containing only one or more carbon atoms and one or more hydrogen atoms.
[0064] The term carbon material, as used herein, refers to one or more forms of carbon. Typically, the carbon material is formed as a particulate solid (or flakes). Examples of carbon materials include the Fullerene allotrope of carbon (see U.S. Pat. No. 11,718,530).
[0065] The term catenated carbon material, as used herein, refers to carbon material comprising carbon molecules bonded in a chain-like manner (see U.S. Pat. No. 11,718,530).
[0066] The term catenated Fullerene, as used herein, refers to fullerene carbon molecules bonded in a chain-like manner (see U.S. Pat. No. 11,718,530).
[0067] The term Fullerene, as used herein, refers to a spherical allotrope of carbon generally known today as C60 fullerene (also buckminsterfullerene originally), consisting of singly unsaturated trigonally substituted carbon atoms all equidistant and equiangular per individual sphere, as in the individual concentric shells of an onion associated with an increased level of electron delocalization around a continuous sphere, and with more thermodynamic stability than that available to the planar graphite or graphene allotrope, but less than that available to the crossene allotrope, where electron delocalization crosses onion shells to incorporate the whole molecular system over that of just the individual concentric shells of a fullerene onion (see U.S. 11,718,530).
[0068] The term downstream, as used herein, in reference to a molten metal process or a molten metal reactor, each as described herein, refers to location of a device that occurs later in the process or the reactor, relative to another device.
[0069] The term upstream, as used herein, in reference to a molten metal process or a molten metal reactor, each as described herein, refers to location of a device that occurs earlier in the process or the reactor, relative to another device.
[0070] The term L.sub.I/W.sub.I ratio, as used here, in reference to a reactor vessel, refers to the ratio of the inner length of the reactor vessel to the inner width of the reactor vessel. Each dimension takes into account the respective dimension of a partition, if present, within the reactor vessel. Note, the inner width of the reactor vessel refers to its largest width, and the inner length of the reactor vessel refers to its largest length.
[0071] The term transfer pump, as used herein, refers to a device used to transfer a stream of molten metal from a molten metal bath to a reactor vessel, to another molten metal bath, or to another device.
[0072] The term circulation pump, as used herein, refers to a device used to circulate a molten metal bath around a reactor vessel, or other device.
[0073] The term product removal assembly, as used herein, refers to an assembly of devices used to remove and/or collect one or more products of one or more chemical reactions from a molten metal process.
[0074] The term collection chamber, as used herein, refer to a device that is used to collect one or more products (for example, one or more carbon materials and/or one or more gases) generated from one or more chemical reactions from a molten metal process.
[0075] The term cyclone separator, as used herein, refers to a device (typically, commercially available) that is used to remove particulate matter (for example, carbon particles) from a gas stream (or liquid stream or vapor stream). This removal is done typically through a vortex separation and/or a centripetal force. Typically, the particulate matter drops into a collection drum or barrel. A gas stream contains one or more gases. A liquid stream and a vapor stream are each similarly defined.
[0076] The term vortex separation, as used herein, refers to a method of separating solid(s) from liquid(s) and/or gas(es), or a method of separating droplets of liquid from a gas stream, each method using rotational effects and gravity.
[0077] The term centripetal force, as used herein, refers to the force necessary to keep an object moving in a curved path, and which force is directed outward toward the center of rotation of the object.
[0078] The term blower, as used herein, refers to a device that pushes out one or more gases by imparting energy to the gas(es) to increase the energy and speed of the gas(es). This energy may provide the motive energy to support a closed circuit recirculating system.
[0079] The term fan, as used herein, refers to a device with rotating blades that creates a current of one or more gases for cooling and/or ventilation.
[0080] The term injection assembly, as used herein, refers to an assembly of one or more components, and which is used to feed a hydrocarbon, or other carbon source, and/or an inert gas into a molten metal bath. The assembly is typically used to feed both the carbon source, as a gas, and an inert gas (for example, argon) into the bath.
[0081] The term injection device, as used herein, refers to an apparatus assemble comprising an inner tube, an inner guard pipe and an outer guard pipe.
[0082] The term injection tip, as used herein, refers to a tube that is partially inserted into the inner tube of the injection device.
[0083] The term injection nozzle, as used herein, refers to an opening that bridges the end of the injection tip with the molten metal bath. Typically, a constant and positive pressure gas flow is generated, prior to submerging the end of the injection tip into the molten metal. Typically, the injection nozzle is formed by a hole within a disk made from a refractory material of certain diameter and thickness.
[0084] The term refractory gasket, as used herein, refers a gasket formed from a composition comprising a majority amount, by weight, of a refractory material. Typically, such a composition comprises 90 wt %, or 95 wt %, or 98 wt %, or 99 wt % of the refractory material, based on the weight of the composition. Typically, such a gasket is used to fill a space by some deformation, and to close and seal gaps.
[0085] The term compressed air, as used herein, refers to air that is kept under a pressure that is greater than atmospheric pressure. Compressed air, just like regular air, comprises hydrogen, oxygen and water vapor. Heat is generated when the air is compressed, and the pressure of the air is increased. When compressed air is released via a small orifice, the gas rapidly cools as it expands, in accordance with Boyles Law, and provides the cooling effect.
[0086] The term injection flow rate, as used herein, refers to the rate at which a gas (for example, a hydrocarbon or argon) is injected into a molten metal.
[0087] The term inert gas, as used herein, refers to a gas that does not change under a given set of conditions. The inert gas, under conditions of interest, does not undergo chemical reactions with other chemical substances, and therefore does not form chemical compounds. Inert gases typically include the noble gases, since such gases often do not react with many substances. Inert gases are used generally to avoid unwanted chemical reactions. These undesirable chemical reactions include, for example, oxidation, catalytic and hydrolysis reactions with the oxygen and water. The term inert gas is context-dependent because an inert gas (for example, several of the noble gases) can be made to react under certain conditions. Purified argon gas is typically the most commonly used inert gas, due to its natural abundance (about 1% argon in air) and low relative cost. The inert gas may also acts as a degassing mechanism to remove the hydrogen from the liquid metal bath.
[0088] The term refractory material, as used herein, refers to a material composition that shows resistance to the temperatures, pressures, and chemicals in a reaction and/or process of interest. Typically, the refractory material is resistant to high temperatures (for example, temperatures melting temperature of a molten metal, or for example, temperatures 1000 F. (538 C.), or 1500 F. (816 C.), or 2000 F. (1093 C.). A refractory material can be used to seal and coat surfaces of a reactor of interest. Refractory materials comprise natural and/or synthetic materials, such as, for example, nonmetallic compounds and minerals, or combinations of such compounds and minerals. Refractory materials include, but are not limited to, boron nitride, alumina, fireclays, bauxite, chromite, dolomite, magnesite, silicon carbide, zirconia, and combinations thereof. An example of a refractory material is BORON NITRIDE PRODUCTS available from Materion.
[0089] The term refractory block, as used herein, refers to a refractory material, used to build (for example, by pouring) a piece of equipment (for example, a plug unit). A refractory block is designed mainly to withstand high heat, but should also usually have a low thermal conductivity to save energy. An example of a refractory block is the refractory material PILCAST AL SHIELD 2765 KK available from Plibrico Company, LLC.
[0090] The term refractory mold, as used herein, refers to a molded apparatus or piece of equipment formed from a refractory material.
[0091] The term gas burner, as used herein, refers to a heating device that operates by burning one or more gases, such as, for example, natural gas. Examples of gas burners include natural gas forced air burners. Typically, gas burners are used in gas fired Reverb Furnaces.
[0092] The term electric resistance heater, as used herein, refers to a device that comprises at least one heating element that converts electrical energy into heat.
[0093] The terms linear flow, or linear flow pattern, each as used herein, refer to a flow regime characterized by parallel flow lines in a molten metal bath.
[0094] The terms partially turbulent flow and partially turbulent flow pattern, as used herein, refer to a flow regime characterized by a combination of linear flow and turbulent flow (the speed of a fluid at a point is continuously undergoing changes in magnitude and direction) in a molten metal bath. A partially turbulent flow is desired to facilitate adequate mixing.
[0095] The term closed-circuit recirculating system, as used herein, refers to a molten metal process or a molten metal reactor, or a reactor component, such as a product collection system, in which each process, reactor, or reactor component is not open to the atmosphere. Typically, such a process, reactor or reactor component comprises piping, ductwork, connections, and flow inducing devices, all involved in transporting, for example, a gas and/or a diffused matter within a gas, from an emission point to a control device and/or to a separation device.
[0096] The term drop tube, as used herein, refers to a device (for example, a pipe) inserted into a process, and where the device serves to redirect and temporarily slow down the movement or velocity flow of matter, to allow particulate or sediment to drop out of the flow path. The drop tube is typically a vertical device that is inserted into a horizontal pipe or tube, and which device collects the dropped out material. Typically, the drop tube has an opening at its bottom that can be opened periodically to collect the trapped (dropped out) material. Downstream of the drop tube, the flow rate typically returns to its normal velocity.
[0097] The term gas recycling device, as used herein, refers to an apparatus used to separate one or more gasses (for example, hydrogen) from an emission stream, and to, independently, collect each gas and/or recycle each gas back to a reactor. It is noted that a recycled inert gas, after the removal of other gases, such as hydrogen, can be recycled to the product removal area and/or the waste input area.
[0098] The term selective permeation membrane, as used herein, refers to a membrane that selectively allows certain molecules and/or ions to pass through it by, for example, a diffusion mechanism, such as a gaseous diffusion. An example of a selective permeation membrane is a SEPURAN NOBLE membrane device available from Evonik. Other examples include palladium membranes and zeolite membranes.
[0099] The phrase a majority of, or similar phrases or terms, as used herein, refer to 50% of the weight, dimension, area, volume, or amount of the subject of interest.
[0100] The phrase recirculation fan in the axial position, as used herein, refers to a recirculation fan situated axially to the flow of the atmosphere moving through the fan.
[0101] The phrase physical piece of equipment, as used herein, refers to a piece of equipment or a device used in a process or reactor of interest.
[0102] The term slag rake assembly, as used herein, refers to an assembly of devices, and which assembly is used to remove slag from the surface of a molten metal bath.
[0103] The term slag rake, as used herein, refers to a device used to remove slag from the surface of a molten metal bath. Typically, the slag rake comprises one or more slag paddle devices, and preferably two slag paddle devices.
[0104] The term slag paddle device as used herein, in reference to a slag rake, refers to the components that make up a functioning slag paddle for the purpose of removing slag from the surface of a molten metal bath.
[0105] The term slag paddle as used herein, in reference to a slag paddle device, refers to a structure used to remove slag from the surface of the molten metal bath. See, for example,
[0106] The term slag, as used herein, refers to a reaction product comprising one or more metal oxides. Such metal oxides are typically formed when oxygen comes into contact with a molten metal bath.
[0107] The phrase central surface area of the slag rake, as used herein, refers to the inner surface of the length of the slag rake. A slag rake, as described herein, has two length sections, where each inner surface faces the inner surface of the other length section. Typically, each inner surface is encompassed within, and surrounded by, an elongated oblong track. See, for example,
[0108] The term insert, as used herein, refers to a structure used to guide each slag paddle to an outlet chamber. See, for example,
[0109] The term outlet chamber, as used herein, refers to a container used to receive slag collected from the surface of a molten metal bath, and which slag is typically transferred along an insert to this chamber. An outlet door is typically located at the bottom of the chamber, which door opens to release the slag into a slag collection chamber, and then recloses to prevent the migration of oxygen into the process closed environment. See, for example,
[0110] The term slag collection container, as used herein, refer to a container that is used to collect slag that falls from an outlet door.
[0111] The term metal oxide, as used herein, refers to a compound comprising oxygen, and at least one metal and/or at least one metalloid. Examples include, but are not limited to, Al.sub.2O.sub.3 (aluminum (III) oxide), AlO (aluminum (II) oxide), Al.sub.2O) (aluminum (I) oxide), and SiO.sub.2 (silicon (IV) oxide).
[0112] The term plug unit, as used herein, refers to a planar structure (for example, top surface area or base surface area >10 the area of a side (or edge) surface). A plug unit is typically formed from a refractory material and/or one or more high temperature resistant metals. The plug unit can acts as a shield to prevent the migration of oxygen to the molten metal bath. It can also provide a surface for the mounting of pumps, heaters, inspection points, thermocouples, and other instruments. The plug unit typically has lifting pad eyes that provide points of attachment for a lifting device, such as a traveling overhead crane. A plug unit is typically readily accessible, and can be readily removed for repair or replacement, or for the repair or replacement of a mounted device, thus reducing the amount of time lost to equipment failure and repair. See, for example,
[0113] The term structural support, as used herein, refers to a component that supports non-variable forces or weights (dead loads) and variable forces or weights (live loads).
[0114] The term partition, as used herein, refers to a structure used to divide or separate portions of a molten metal bath. See, for example,
[0115] The phrase reactor is in operation, and similar phrases, as used herein, refer to the injection of a carbon source into a molten metal, the subsequent reaction of the carbon source with the molten metal bath, and, optionally, the separation and/or collection of the reaction product(s).
[0116] The term headspace, as used herein, refers to the atmosphere above the molten metal bath surface.
[0117] The term makeup molten metal, as used herein, refers to the molten metal that is used to replenish the amount of the molten metal bath consumed in the formation of slag and/or other reaction(s).
[0118] The term sunken pit, as used herein, refers to a pit that comprises a base that is lower, on all sides, than the surrounding floor area. The sunken pit may serve as a catch basin for the molten metal in the case of a leak, such as, for example, a leak in a reactor vessel. The pit may also serves as an annulus space for ventilation under the reactor, to keep the adjacent area under the reactor at a cooler temperature.
[0119] The Temperature (T1) of the molten metal in the reactor vessel, as used herein, refers to the average temperature of the temperatures from four or more thermocouples located at various positions in the molten metal bath.
[0120] The term on-line feed system, as used herein, refers to the apparatus (for example, piping components and gauges) used to feed, to a reactor, a chemical (for example a carbon source or an inert gas) from a manufacturing plant that produces the chemical.
[0121] The term gas back pressure, as used herein in reference to a gas flow, through a gas flow meter, refers to the pressure measured at the outlet side of the gas flow meter.
Listing of Some Reactor and Process Features
[0122] A] A molten metal reactor comprising at least the following components a) through c): [0123] a) a reactor vessel comprising a molten metal bath, [0124] b) an injection assembly, and [0125] c) a product removal assembly. [0126] B] The molten metal reactor of A] above, wherein the reactor further comprises a partition located within the reactor vessel. [0127] C] The molten metal reactor of A] or B] above, wherein the ratio of the width of the partition to the inner width of the reactor vessel is 0.20, or 0.30, or 0.40, or 0.50 and/or 0.80, or 0.70, or 0.60. Note, the width of the partition refers to its largest width, and the inner width of the reactor vessel refers to its largest width. [0128] D] The molten metal reactor of any one of A]-C] (A] through C]) above, wherein the ratio of the length of the partition to the inner length of the reactor vessel is 0.20, or 0.30 inch, or 0.40, or 0.50 and/or 0.80, or 0.70, or 0.60. Note, the length of the partition refers to its largest length, and the inner length of the reactor vessel refers to its largest length. [0129] E] The molten metal reactor of A] or B] above, wherein the ratio of the width of the partition to the inner width of the reactor vessel is 0.20, or 0.25, or 0.30 and/or 0.50, or 0.45, or 0.40. [0130] F] The molten metal reactor of A] or B] or E] above, wherein the ratio of the length of the partition to the inner length of the reactor vessel is 0.50, or 0.60, or 0.70 and/or 0.90, or 0.85, or 0.80. [0131] G] The molten metal reactor of any one of A]-F] above, wherein the reactor further comprises 1 plug unit(s), or 2 plug units. [0132] H] The molten metal reactor of G] above, wherein each plug unit is used to seal in a positive pressure, inert gas purge, to reduce the amount of oxygen that can leak into the reactor. [0133] I] The molten metal reactor of G] or H] above, wherein each plug unit is removable. [0134] J] The molten metal reactor of any one of G]-H] above, wherein each plug unit can be moved by a lifting device (such as, for example, a traveling overhead crane). [0135] K] The molten metal reactor of any one of G]-J] above, wherein the bottom surface of each plug unit is inserted into the molten metal bath. [0136] L] The molten metal reactor of any one of G]-K] above, wherein the bottom surface of each plug unit is independently inserted into the molten metal bath, at a depth of 0.20 inch (0.51 cm), or 0.30 inch (0.76 cm), or 0.40 inch (1.0 cm), or 0.50 inch (1.3 cm), as measured from the bottom surface of the plug unit. [0137] M] The molten metal reactor of any one of G]-L] above, wherein the bottom surface of each plug unit is independently inserted into the molten metal bath, at a depth of 3.0 in (7.62 cm), or 2.5 in (6.4 cm), or 2.0 in (5.1 cm), or 1.5 in (3.8 cm), as measured from the bottom surface of the plug unit. [0138] N] The molten metal reactor of any one of G]-M] above, wherein each plug unit is over an open surface of the reactor vessel when the reactor is in operation. [0139] O] The molten metal reactor of any one of G]-N] above, wherein each plug unit may provide structural support for one or more other pieces of equipment. [0140] P] The molten metal reactor of any one of A]-O] above, wherein the injection assembly is located on a plug unit. [0141] Q] The molten metal reactor of any one of A]-P] above, wherein the injection assembly comprises 1 injection device(s), or 2 injection devices, and further 2 injection devices. [0142] R] The molten metal reactor of Q] above, wherein at least one injection device is used to inject at least one carbon source into the molten metal bath, and further the at least one carbon source has a purity 90.0 vol %, or 92.0 vol %, or 94.0 vol %, or 96.0 vol %, or 98.0 vol %, or 99.0 vol % and/or 100.0 vol %, based on the volume of the carbon source. [0143] S] The molten metal reactor of R] above, wherein the at least one carbon source is at least one hydrocarbon. [0144] T] The molten metal reactor of S] above, wherein the at least one hydrocarbon has a purity 90.0 vol %, or 92.0 vol %, or 94.0 vol %, or 96.0 vol %, or 98.0 vol %, or 99.0 vol % and/or 100.0 vol %, based on the volume of the hydrocarbon. [0145] U] The molten metal reactor of S] or T] above, wherein the at least one hydrocarbon is acetylene or methane; and further acetylene. [0146] V] The molten metal reactor of any one of Q]-U] above, wherein at least one injection device is used to inject at least one inert gas into the molten metal bath. [0147] W] The molten metal reactor of V] above, wherein the at least one inert gas has a purity 99.0 vol % and/or 100.0 vol %, based on the volume of the inert gas. [0148] X] The molten metal reactor of V] or W] above, wherein the at least one inert gas is argon. [0149] Y] The molten metal reactor of any one of Q]-X] above, wherein at least one injection device is located on a plug unit, and further on the same plug unit on which the injection assembly is located. [0150] Z] The molten metal reactor of Y] above, wherein two injection devices are located on the plug unit. [0151] A2] The molten metal reactor of any one of Q]-Z] above, wherein each injection device comprises the following components: i) an inner tube, ii) an inner guard pipe, iii) an outer guard pipe. [0152] B2] The molten metal reactor of A2] above, wherein the inner tube is wrapped with a tubing, and further spiral wrapped with the tubing. For example, see
[0232] D5] The molten metal reactor of any one of A]-CS] above, wherein slag is produced in the reactor vessel; and further the slag rises to the surface of the molten metal bath. [0233] E5] The molten metal reactor of D5] above, wherein the slag comprises one or more metal oxides. [0234] F5] The molten metal reactor of any one of A]-E5] above, wherein the reactor further comprises a slag rake assembly. [0235] G5] The molten metal reactor of F5] above, wherein the slag rake assembly is used to remove slag from the surface of the molten metal bath. [0236] H5] The molten metal reactor of F5] or G5] above, wherein the slag rake assemble comprises a slag rake. [0237] I5] The molten metal reactor of H5] above, wherein the slag rake comprises at least one slag paddle device that comprises a slag paddle and a solid rod, and further the slag rake comprises two slag paddle devices. [0238] J5] The molten metal reactor of 15] above, wherein the solid rod is formed from a composition comprising at least one metal. [0239] K5] The molten metal reactor of 15] or J5] above, wherein a portion of the slag paddle is submerged beneath the surface of the molten metal bath, to collect the slag on the surface of the bath. [0240] L5] The molten metal reactor of any one of 15]-K5] above, wherein each slag paddle device travels around a central surface area of the slag rake, when the reactor is in operation. [0241] M5] The molten metal reactor of any one of 15]-L5] above, wherein a chain and sprocket mechanism or a pully mechanism is used to move the slag paddle device around a track on the slag rake. [0242] N5] The molten metal reactor of any one of 15]-M5] above, wherein the molten metal reactor further comprises an insert, an outlet chamber, and a slag collection container. [0243] O5] The molten metal reactor of N5] above, wherein the outlet chamber comprises an outlet door. [0244] P5] The molten metal reactor of N5] or 05] above, wherein the slag paddle transports the slag along the insert to the outlet chamber. [0245] Q5] The molten metal reactor of 05] or P5] above, wherein the outlet door is located at the bottom of the outlet chamber. [0246] R5] The molten metal reactor of any one of OS]-Q5] above, wherein the outlet door opens when in contact with the slag, and the slag drops into the slag collection container. [0247] S5] The molten metal reactor of any one of F5]-RS] above, wherein there is no headspace above the molten metal bath, apart from the area under the collection chamber and the area under the slag rake assembly. [0248] T5] The molten metal reactor of any one of A]-S5] above, wherein the reactor further comprises a lauder makeup vessel and a transfer pump. [0249] U5] The molten metal reactor of T5] above, wherein the lauder makeup vessel and the transfer pump are used to supply makeup molten metal to the molten metal bath in the reactor vessel. [0250] V5] The molten metal reactor of any one of R4]-U5] above, wherein the hydrogen is separated and collected. [0251] W5] The molten metal reactor of V5] above, wherein the hydrogen is separated using a device comprising a selective permeation membrane. [0252] X5] The molten metal reactor of V5] or W5] above, wherein the hydrogen flows through a vent in a collection chamber, and further the collection chamber of the product removal assembly. [0253] Y5] The molten metal reactor of any one of R]-X5] above, wherein the at least one carbon source is fed to the reactor using an on-line feed system. [0254] Z5] The molten metal reactor of any one of V]-Y5] above, wherein the at least one inert gas is fed to the reactor using an on-line feed system. [0255] A6] The molten metal reactor of any one of U4]-Z5] above, wherein the product removal assembly is used to remove the one or more carbon materials and the one or more gases, each liberated from the molten metal bath; further to remove a majority, by weight, of each of the one or more carbon materials and the one or more gases, each liberated from the molten metal bath; and the product removal assembly comprises 1 cyclone separator(s), or 2 or more cyclone separators, or 3 or more cyclone separators; and wherein each cyclone separator is used to separate the one or more carbon materials from the one or more gases. [0256] A7] A process to prepare a composition comprising a carbon material, the process comprising adding a carbon source to the molten metal reactor of any one of A]-A6] above. [0257] B7] The process of A7] above, wherein the carbon material is present in an amount 80 wt %, or 85 wt %, or 90 wt %, or 92 wt %, or 94 wt %, or 96 wt %, 98 wt %, or 99 wt %, based on the weight of the composition and/or present in an amount 100 wt %, based on the weight of the composition. [0258] C7] The process of A7] or B7] above, wherein the carbon material is a catenated carbon material. [0259] D7] The process of C7] above, wherein the catenated carbon material is a catenated fullerene. [0260] E7] A composition comprising a carbon material, and wherein the composition is formed using the molten metal reactor of any one of A]-A6] above. [0261] F7] The composition of E7] above, wherein the carbon material is present in an amount 80 wt %, or 85 wt %, or 90 wt %, or 92 wt %, or 94 wt %, or 96 wt %, 98 wt %, or 99 wt %, based on the weight of the composition and/or present in an amount 100 wt %, based on the weight of the composition. [0262] G7] The composition of E7] or F7] above, wherein the carbon material is a catenated carbon material. [0263] H7] The composition of G7] above, wherein the catenated carbon material is a catenated fullerene. [0264] I7] An article comprising at least one component formed from the composition of any one of E7]-H7] above. [0265] J7] A composition comprising a carbon material, and wherein the composition is formed from the process of any one of A7]-D7] above. [0266] K7] The composition of J7] above, wherein the carbon material is present in an amount 80 wt %, or 85 wt %, or 90 wt %, or 92 wt %, or 94 wt %, or 96 wt %, 98 wt %, or 99 wt %, based on the weight of the composition and/or present in an amount 100 wt %, based on the weight of the composition. [0267] L7] The composition of J7] or K7] above, wherein the carbon material is a catenated carbon material. [0268] M7] The composition of L7] above, wherein the catenated carbon material is a catenated fullerene. [0269] N7] An article comprising at least one component formed from the composition of any one of J7]-M7] above.
EXPERIMENTAL
[0270] A molten bath reaction may be run in accordance with, for example,
[0271] Note, a molten aluminum bath may be used, and the molten metal bath is already established, and in a phase 3 operational mode. Composition of molten metal bath is 99 wt % Al, based on the weight of the molten metal. The reagents are as follows:
[0272] Acetylene gas with a purity of 99 vol %, based on the volume of acetylene gas used. See, for example, Airgas products.
[0273] Argon gas with a purity of 99 vol %, based on the volume of argon gas used. See, for example, Airgas products.
[0274] Injection flow rate of the acetylene gas of 10 L/min, at a pressure (gas back pressure) of about 4.0 psi or higher.
[0275] Injection flow rate of the argon gas of 10 L/min, at a pressure gas back pressure of about 4.0 psi or higher. The reactor is purged with argon gas, and this purge remains throughout the operation of the reactor.
[0276] Injection assembly see
[0277] The ratio of the volume of the argon injected into the molten metal bath (V.sub.AR) to the volume of acetylene injected into the molten metal bath (VAC) or VAR/VAC =1.0.
[0278] Description of partition-longitudinal partition that is centered in the reaction vessel.
[0279] The L.sub.I/W.sub.I ratio of reactor vessel (including the partition) =2.5.
[0280] The exposed surfaces of the reactor vessel are covered with one or more plug units. Each component of the reactor that comes into contact with the molten metal bath is independently coated with a refractory, such as boron nitride.
[0281] At least one circulation pump.
[0282] Four electric resistance heater, each generating 17,000 kilowatts of electrical power. The heating element of each heater is inserted into the molten metal bath to minimize heat dissipation to areas outside the reactor vessel.
[0283] Product removal assemblysee
[0284] Temperature (T1) of the molten metal in the reactor vessel is around 1450 F. to 1500 F. (788 C. to 816 C.). Temperature T1 is the average temperature of the temperatures noted on the following thermocouples: a) four thermocouples located on each corner of the reactor vessel, b) one thermocouple located downstream from the injection port, and c) two thermocouples located within the bath, near the inlet and outlet, respectively, of the circulation pump.
[0285] The speed the molten metal bath travels around the of the reactor vessel =0.2 RPM (one circuit of the total inventory of the molten metal in the reactor vessel in 1 minute.
[0286] As discussed, plug units are used to cover all the open areas above the molten metal bath. Note a slag rake assembly can be used to remove slagsee
[0287] The carbon material(s) produced from the reaction of acetylene with the molten metal will be collected in the collection barrels and in the drop tubes (see
[0288] Note, each thermocouple output will be recorded with a video display of the operating parameters. Operating set points will be established, and the data collected will control the power output of the heaters, pumps and fans used, to maintain the molten aluminum at the desired temperature.
[0289] The above described embodiments are intended to illustrate the principles of the reactors and processes described herein, but not to limit the scope of the invention. Various other embodiments and modifications to these embodiments may be made by those skilled in the art, without departing from the scope of the following claims.