Patent Application
20240416307
Embodiments of the present disclosure generally relate to methods and systems for loading catalysts, and particularly to loading catalysts for testing in pilot reactors.
Catalysts play an important role in many refinery and reactor processes, with new catalyst compositions being consistently developed. Accordingly, pilot plant evaluation of these catalysts is an important step before broader implementation and scale-up for use in commercial reactors.
For example, in typical hydroprocessing trickle-bed reactors may be used, in which a liquid phase and a gas phase flow concurrently downward through a fixed bed of catalyst particles while the reaction with the catalyst takes place. Accordingly, pilot plant processes may mimic these trickle-bed reactors by vertically loading ‘packing’ a catalyst in a metal tube, then loading that metal tube into a system that flows a testing feed across the metal tube to test the catalyst's performance. Metal tubes are used due to the severe conditions (temperature and/or pressure) of most pilot plant processes. However, typical catalyst loading procedures may introduce multiple sources of error through void spaces within the catalyst pack, which in turn may cause channeling of the feedstock throughout these void spaces.
One traditional solution to the void space problem is to additionally add inert material of a relatively smaller size than the loaded catalyst, which ideally will ‘gap fill’ the void spaces between catalyst particles. However, visual confirmation of this gap fill is ordinarily impossible because the metal tubes used are not transparent. Glass and similar materials are transparent, but do not normally contain the properties necessary for use in reactor conditions. Accordingly, methods and apparatuses are desired for loading catalysts for use in pilot reactors while also being able to visually observe the catalyst loading.
Consequently, described herein are integrated methods and systems for loading catalysts, while providing the aforementioned benefits. Particularly, visual observation and confirmation of proper catalyst loading may be affected by loading the catalyst in an optically transparent tube coated by wax. The optically transparent tube is coupled to a metal tube, with an internal cavity defined by the two tubes separated by a horizontal divider. The loaded catalyst may then be transferred to the metal tube from the optically transparent tube by removal of the horizontal divider and displacement of the loaded catalyst. The layer of wax may help move the loaded catalyst as one mass, thereby limiting the shifting of catalyst and inert materials within. Methods of displacement may include melting the wax layer surrounding the loaded catalyst, thereby causing the loaded catalyst to slide down into the metal tube, but may also include compressive force to move the loaded catalyst to the metal tube or differential pressure from the optically transparent tube to the metal tube.
In accordance with an embodiment herein, a method of loading a catalyst includes providing a catalyst loading apparatus, the catalyst loading apparatus including: an optically transparent tube having an interior surface and an exterior surface, a metal tube having an interior surface and an exterior surface, removably coupled to, and disposed below the optically transparent tube, wherein the optically transparent tube and the metal tube together define a cavity extending from a top surface of the optically transparent tube to a bottom surface of the metal tube, a horizontal divider including a horizontal divider shaft and a plate coupled to a distal end of the horizontal divider shaft, wherein the horizontal divider is positioned within the interior surface of the optically transparent tube, the metal tube, or at least partially within both, and the plate is configured to block the cavity, and a leveling device including a leveling device shaft and a disc coupled to a distal end of the leveling device shaft, the disc sized to be inserted into the cavity. The method also includes adding a first inert material to the optically transparent tube to form a first layer including the first inert material; adding a catalyst to the optically transparent tube to form a second layer including the catalyst disposed above the first layer; adding a second inert material to the optically transparent tube at least until substantially no void space is observed in the second layer, the second inert material having a lesser diameter than the first inert material and the catalyst; inserting the disc of the leveling device into the cavity from the top surface of the optically transparent tube; contacting the disc of the leveling device against the second layer including the catalyst; and displacing the leveling device, the first layer, the second layer, and the horizontal divider into the metal tube.
In accordance with another embodiment herein, a method for loading a catalyst includes providing a catalyst loading apparatus, the catalyst loading apparatus including an optically transparent tube having an interior surface and an exterior surface, a metal tube having an interior surface and an exterior surface, removably coupled to, and disposed below the optically transparent tube, wherein the optically transparent tube and the metal tube together define a cavity extending from a top surface of the optically transparent tube to a bottom surface of the metal tube, a horizontal divider including a horizontal divider shaft and a plate coupled to a distal end of the horizontal divider shaft, wherein the horizontal divider is positioned within the interior surface of the optically transparent tube, the metal tube, or at least partially within both, and the plate is configured to block the cavity, and a leveling device including a leveling device shaft and a disc coupled to a distal end of the leveling device shaft, the disc sized to be inserted into the cavity. The method also includes coating the interior surface of the optically transparent tube, the interior surface of the metal tube, a horizontal divider plate top surface, or combinations thereof with a first wax; adding a first inert material to the optically transparent tube to form a first layer including the first inert material; adding a catalyst to the optically transparent tube to form a second layer including the catalyst disposed above the first layer; adding a second inert material to the optically transparent tube at least until substantially no void space is observed in the second layer, the second inert material having a lesser diameter than the first inert material and the catalyst; adding additional first inert material to the optically transparent tube prior to inserting the leveling device to form a third layer including the first inert material disposed above the second layer; and adding a second wax to the optically transparent tube at least until the second wax is observed to coat the horizontal divider plate top surface inserting the disc of the leveling device into the cavity from the top surface of the optically transparent tube; contacting the disc of the leveling device against the third layer; displacing the leveling device, the first layer, the second layer, the third layer, and the horizontal divider into the metal tube; removing the leveling device from the optically transparent tube; decoupling the optically transparent tube from the metal tube; coupling a cover to a top surface of the metal tube, the cover including a screen; inverting the catalyst loading apparatus; and removing the horizontal divider from the metal tube.
In accordance with yet another embodiment herein, a system for loading a catalyst includes one or more catalyst loading assemblies, the one or more catalyst loading assemblies including an optically transparent tube having an interior surface and an exterior surface, a metal tube having an interior surface and an exterior surface, removably coupled to, and disposed below the optically transparent tube, wherein the optically transparent tube and the metal tube together define a cavity extending from a top surface of the optically transparent tube to a bottom surface of the metal tube, and a horizontal divider including a shaft and a plate coupled to a distal end of the shaft, wherein the horizontal divider is positioned within the interior surface of the optically transparent tube, the metal tube, or at least partially within both, has the shaft proximal the bottom surface of the metal tube, has the plate proximal the top surface of the optically transparent tube, and is configured to block the cavity. The system also includes at least one coupling mechanism removably coupled to the exterior surface of the optically transparent tube, the metal tube, or both; and at least one arm coupled to the at least one coupling mechanism and operable to suspend the at least one catalyst loading apparatus in a vertical position with the at least one coupling mechanism.
Additional features and advantages of the embodiments described herein will be set forth in the detailed description which follows, and in part will be readily apparent to those skilled in the art from that description or recognized by practicing the embodiments described, including the detailed description and the claims which are provided infra.
The following detailed description of specific embodiments of the present disclosure can be best understood when read in conjunction with the following drawings in which:
Reference will now be made in greater detail to various embodiments, some embodiments of which are illustrated in the accompanying drawings. Whenever possible, the same reference numerals will be used throughout the drawings to refer to the same or similar parts.
Embodiments of the present disclosure generally relate to methods and systems for loading catalysts, and particularly to loading catalysts for testing in pilot reactors.
As used herein, a “catalyst” refers to any substance that increases the rate of a specific chemical reaction. Catalysts described in this disclosure may be utilized to promote various reactions, such as, but not limited to, hydrotreating, hydrocracking, hydroprocessing, hydrodemetalization, hydrodesulfurization, hydrodenitrogenation, aromatic methylation, disproportionation, dealkylation, transalkylation, diaromatic dearylation, and isomerization.
As used herein, “optically transparent” means an average transmittance of 70% or more in the wavelength range of 400 nm to 700 nm through a 1.0 mm thick piece of a material. In embodiments, an optically transparent material may have an average transmittance of 75% or more, 80% or more, 85% or more, or 90% or more in the wavelength range of 400 nm to 700nm through a 1.0 mm thick piece of the material. The average transmittance in the wavelength range of 400 nm to 700 nm is calculated by measuring the transmittance of all whole number wavelengths from 400 nm to 700 nm and averaging the measurements.
Referring initially to
As previously stated, the catalyst loading apparatus 100 may include the first horizontal divider 118. The first horizontal divider 118 may be removably coupled to and disposed below the optically transparent tube 104. The first horizontal divider 118 may also be removably coupled to and disposed above the metal tube 108. Accordingly, when removably coupled together, the optically transparent tube 104, the metal tube 108, and the first horizontal divider 118 may together define a cavity 101 extending from the top surface 150a of the optically transparent tube 104 to the bottom surface 151b of the metal tube 108. The cavity 101 may in turn be configured to provide an unobstructed fluid pathway through the catalyst loading apparatus 100.
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In embodiments, the catalyst loading apparatus 100 may further include a screen 127 removably coupled to the metal tube 108 at the metal tube 108′s bottom surface 151b through one of the coupling mechanisms previously stated. The screen may be operable to permit fluid flow out of the catalyst loading apparatus 100, but block solid material such as a catalyst or inert material, as described in further detail infra.
In embodiments, the catalyst loading apparatus 100, including the optically transparent tube 104, the first horizontal divider 118, the metal tube 108 or combinations thereof, may be sized to fit in traditional pilot plant reactors for testing catalyst compositions. For example, in one non-limiting embodiment, an interior diameter of the interior surfaces 105, 109, 120 of the catalyst loading apparatus 100 may be from 1 centimeter (cm) to 15 cm, such as from 0.1 cm to 0.5 cm, from 0.5 cm to 1 cm, from 1 cm to 2 cm, from 2 cm to 4 cm, from 4 cm to 8 cm, from 8 cm to 12 cm, from 12 cm to 14 cm, from 14 cm to 15 cm, from 15 cm to 20 cm, from 20 cm to 50 cm, or any combination of ranges or smaller range therein, such as from 0.1 cm to 50 cm. Similarly. in embodiments, the length of the optically transparent tube 104, the first horizontal divider 118, the metal tube 108, or combinations thereof, may be from 0.1 meters (m) to 10 meters, such as from 0.01 m to 0.05 m, from 0.05 m to 0.1 m, from 0.1 m to 0.2 m, from 0.2 m to.5 m, from 0.5 m to 1 m, from 1 m to 4 m, from 4 m to 8 m, from 8 m to 9 m, from 9 m to 10 m, from 10 m to 15 m, from 15 m to 25 m, or any combination of ranges or smaller range therein, such as from 0.01 m to 25 m.
The optically transparent tube 104 may be composed of any one of a number of materials known to be optically transparent. For example, and in embodiments, the optically transparent tube may include plexiglass, glass, or any polymeric material that is optically transparent, such that the internal contents of the optically transparent tube may be visually observed by an individual or optical device. The metal tube 108 may be composed of any one of a number of materials capable of withstanding pilot plant reactor conditions. For example, and in embodiments, the metal tube may include steel or metallic alloys including nickel, molybdenum, chromium, or combinations thereof.
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In at least one embodiment, the second horizontal divider 118′ and the leveling device 128 may be configured to be inserted through, respectively, the metal tube bottom surface 151b and the optically transparent tube's top surface 150a. The second horizontal divider 118 may be orientated such that the plate 162 is proximal the optically transparent tube's top surface 150a. In other words, the plate 162 may be nearer to the optically transparent tube's top surface 150a than the horizontal divider shaft 160. Likewise, the horizontal divider shaft 160 may be proximal the metal tube's bottom surface 151b.
Accordingly, as illustrated in
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The at least one heating element 116 may heat the optically transparent tube 104. the first horizontal divider 118, the metal tube 108, or combinations thereof through any manner understood in the art, such as, but not limited to, electrically inductive heating. Accordingly, without being limited by theory, the heating element may be electrically coupled to a power source operable to provide an electric current through the heating element, and thereby generate heat form the heating element.
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Alternatively or additionally, the at least one coupling mechanism 113 may include an open end, i.e. the at least one coupling mechanism 113 may not entirely circumferentially surround the catalyst loading apparatus 100. Accordingly, the at least one coupling mechanism may define a window 115, thereby allowing unobstructed observation of the window defined portion of the catalyst loading apparatus 100. As shown in coupling mechanism 113B as compared to coupling mechanism 113C, the window 115 may be larger (wider) in some embodiments than in others.
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The process may first include providing the catalyst loading apparatus. The process may then include coating the interior surface 105, the interior surface 109, or both, with a first wax. As shown in
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The first inert material 136 may have a particle diameter of from 5 mesh to 40 mesh, such as from 5 mesh to 10 mesh, from 10 mesh to 20 mesh, from 20 mesh to 30 mesh, from 30mesh to 40 mesh, or any combination of ranges or smaller range therein. The second inert material 144 may have a particle diameter of from 50 mesh to 100 mesh, such as from 50 mesh to 60 mesh, from 60 mesh to 70 mesh, from 70 mesh to 90 mesh, from 90 mesh to 100 mesh, or any combination of ranges or smaller range therein. The first inert material 136, the second inert material 144, or both may include silicon carbide, glass beads, sand, or combinations thereof.
For catalyst loading apparatus 100, the method may then include actuating the gate 121 of the first horizontal divider 118 into the opened position. As previously described, actuating the gate 121 to the opened position may operate to create an unobstructed fluid pathway within the catalyst loading apparatus 100 along the cavity 101. After the gate 121 is in the open position, the first and second layers 137/141 may be displaced into the metal tube 108 from the optically transparent tube 104. The method may then involve removing the first horizontal divider 118 from the catalyst loading apparatus 100.
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Moreover, for catalyst loading apparatus 100′, compressing of the catalyst 140 of the second layer 141 may operate to displace the first and second layers, and thereby the second horizontal divider 118′, into the metal tube 108. Particularly, as previously stated, the insertion of the leveling device 128 in combination with the second horizontal divider 118′ for catalyst loading apparatus 100′ may operate to sandwich the first and second layers, or the first through third layers as discussed below, between the leveling device 128 and the second horizontal divider 118′, minimizing disruption of the relative orientation of the layers.
The method may also include agitating or vibrating the catalyst loading apparatus contemporaneously with the addition of the catalyst 140, the addition of the second inert material 144, or both, such as with the settling device discussed supra.
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Without being limited by theory, the addition of the second wax may help to further stabilize the layers relative positions while being displaced to the metal tube 108. The addition of the second wax may also additionally help protect the layers from exposure to external substances and preserve the catalyst 140 before use.
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It is noted that recitations in the present disclosure of a component of the present disclosure being “operable” or “sufficient” in a particular way, to embody a particular property, or to function in a particular manner, are structural recitations, as opposed to recitations of intended use. More specifically, the references in the present disclosure to the manner in which a component is “operable” or “sufficient” denotes an existing physical condition of the component and, as such, is to be taken as a definite recitation of the structural characteristics of the component.
It is also noted that terms like “preferably,” “commonly,” and “typically,” when utilized herein, are not utilized to limit the scope of the claimed invention or to imply that certain features are critical, essential, or even important to the structure or function of the claimed invention. Rather, these terms are merely intended to identify particular aspects of an embodiment of the present disclosure or to emphasize alternative or additional features that may or may not be utilized in a particular embodiment of the present disclosure.
It is noted that one or more of the following claims utilize the term “wherein” as a transitional phrase. For the purposes of defining the present invention, it is noted that this term is introduced in the claims as an open-ended transitional phrase that is used to introduce a recitation of a series of characteristics of the structure and should be interpreted in like manner as the more commonly used open-ended preamble term “comprising.”
Having described the subject matter of the present disclosure in detail and by reference to specific embodiments, it is noted that the various details disclosed in the present disclosure should not be taken to imply that these details relate to elements that are essential components of the various embodiments described in the present disclosure. Further, it will be apparent that modifications and variations are possible without departing from the scope of the present disclosure, including, but not limited to, embodiments defined in the appended claims.
The singular forms “a”, “an” and “the” include plural referents, unless the context clearly dictates otherwise.
Throughout this disclosure ranges are provided. It is envisioned that each discrete value encompassed by the ranges are also included. Additionally, the ranges which may be formed by each discrete value encompassed by the explicitly disclosed ranges are equally envisioned.
As used herein and in the appended claims, the words “comprise,” “has,” and “include” and all grammatical variations thereof are each intended to have an open, non-limiting meaning that does not exclude additional elements or steps.
As used herein, terms such as “first” and “second” are arbitrarily assigned and are merely intended to differentiate between two or more instances or components. It is to be understood that the words “first” and “second” serve no other purpose and are not part of the name or description of the component, nor do they necessarily define a relative location, position, or order of the component. Furthermore, it is to be understood that the mere use of the term “first” and “second” does not require that there be any “third” component, although that possibility is contemplated under the scope of the present disclosure.
