1. Field of the Invention
The present invention relates to an apparatus and method for processing of a material sample, such as a catalyst.
2. Description of the Related Art
Before a material is selected for use in a commercial application, for example catalysts for hydrocarbon reactions in petroleum refining, a great number of materials may be examined for use in the envisioned application. A large number of material compositions may be synthesized, processed and screened while under consideration as candidates.
The traditional approach to the processing of new material has been a sequential one. One new potential material undergoes a process step in a vessel. Upon completion of the process step, the one material is removed from the vessel and a second material is loaded. The process is repeated on the freshly loaded material. The process is repeated sequentially for each of the materials. Not only is this approach drawn out for a single process step, but the time requirement is compounded by multiple process steps which may require multiple process vessels. Overall, processing of a plurality of new material formulations is a lengthy process at best.
One method that has been employed for individual processing steps is to take a combinatorial approach. Combinatorial chemistry has dealt mainly with the synthesis of new compounds. For example, U.S. Pat. No. 5,612,002 and U.S. Pat. No. 5,766,556 teach an apparatus and a method for simultaneous synthesis of multiple compounds. Akporiaye, D. E.; Dahl, I. M.; Karlsson, A.; Wendelbo, R. Angew Chem. Int. Ed. 1998, 37, 9-611 disclose a combinatorial approach to the hydrothermal synthesis of zeolites, see also WO 98/36826.
Combinatorial approaches have also recently been used for the evaluation and screening of catalysts; see for example commonly assigned U.S. Pat. Nos. 6,342,185 and 6,368,865 and U.S. patent applications Ser. Nos. 10/095,395, 10/095,879 and 10/095,934.
A system for the parallel treatment of a plurality of materials is also disclosed in the commonly assigned patent applications having Attorney Docket Numbers 105279 and 105397, filed contemporaneously herewith, the disclosures of which are incorporated herein by reference.
Efforts have been made to expedite processing of a plurality of materials by placing a small amount of each material into a corresponding number of containers and then processing each container. Attempts also have been made to use several containers simultaneously in an array in order to analyze samples. An example of simultaneously using multiple containers is disclosed in U.S. Pat. No. 4,766,082 and in the Argonaut Endeavor apparatus.
The use of multiple containers eliminates the need to load and unload a single container several times. However, the use of multiple containers still has required manual manipulation of each container, which is a slow and clumsy process, particularly when each individual material, and hence each individual container, must undergo a plurality of sequential process steps. Moreover, it may be desired to vary the process steps, which adds further complication and time.
What is needed is an apparatus and method to automate and speed up the processing of materials in order to improve efficiency of the material preparation and examination process.
The present invention allows for the rapid movement of material samples by using a processing device to position one or more cartridges from a series of cartridges into the processing device for preparation or examination of a material contained within the cartridge. In accordance with the present invention, a novel and improved apparatus is provided for contacting a plurality of solid material samples with fluid in a series of cartridges. The inventive apparatus includes a processing device for passing fluid through an interior volume of a cartridge, the processing device having a feed port and an effluent port and the cartridge having an inlet and an outlet, at least one cartridge position controller for positioning the cartridge between the feed port and the effluent port and for removing the cartridge from between the feed port and the effluent port, a first seal for sealing between the feed port and the cartridge inlet, and a second seal for sealing between the effluent port and the cartridge outlet.
Also in accordance with the present invention, a novel and improved method is provided for processing material. The inventive method includes the steps of loading material to be processed into a cartridge, wherein the cartridge includes an inlet and an outlet, positioning the cartridge between a feed port and an effluent port, sealing between the cartridge inlet and the feed port and between the cartridge outlet and the effluent port, flowing fluid through the cartridge, and releasing the cartridge from between the feed port and the effluent port.
These and other objects, features and advantages are evident from the following description of an embodiment of the present invention, with reference to the accompanying drawings.
A novel and improved material processing device 10 for processing materials 2 is shown in
Each processing device 10 includes a feed section 12 having a feed port 46, an effluent section 14 having an effluent port 56 and a cartridge station 18 located between feed section 12 and effluent section 14. A cartridge 16 for holding a small sample of material 2 is placed in cartridge station 18, between feed port 46 and effluent port 56, as is shown in
Processing device 10 can be used for several types of catalyst or material process steps. Examples of process steps for which process device 10 can be used include preparation steps, pre-treatment steps, treatment steps (such as heat treatment), finishing steps, and screening steps.
A certain set of process conditions define a process step, such as fluid flow rates and composition or temperature. Therefore two operations define different process steps if they process material 2 under different process conditions.
For the example of heat treatment of an inorganic catalyst, in one method processing device 10 can be operated with fluid flow rates between about 0.1 cm3/min to about 1000 cm3/min, preferably between about 0.5 cm3/min and about 25 cm3/min. The fluid can also be heated, as described below, to temperatures between room temperature of about 20° C., to high temperatures of about 1000° C., and preferably between about 300° C. and about 800° C. Other process conditions that can be altered in processing device 10 include materials 2 being processed, and processing fluids used to process materials 2.
Preferred materials 2 that can be processed within processing device 10 include inorganic catalysts, such as metallic catalysts used in the petrochemical industry, metals, and other inorganic materials which may undergo one or more process steps before the material has certain desired properties.
Examples of catalysts that may be processed using the present invention include those effective in a wide variety of hydrocarbon conversion processes such as cracking, hydrocracking, alkylation of both aromatics and isoparaffins, isomerization, polymerization, reforming, dewaxing, hydrogenation, dehydrogenation, transalkylation, dealkylation, hydration, dehydration, hydrotreating, hydrodenitrogenation, hydrodesulfurization, methanation, ring opening, and syn-gas shift processes. Specific examples are discussed in H. Pines, The Chemistry Of Catalytic Hydrocarbon Conversions, Academic Press (1981).
Examples of process fluids being fed to processing device 10 include pure components, such as pure hydrogen gas, oxygen gas, H2O gas and H2O liquid, or mixtures of components, such as half nitrogen gas and half air, or a mixture of hydrochloric acid and water (aqueous HCl).
Processing device 10 provides a flow of a process fluid through a sample of material 2 in order to perform a particular process step. The process fluid feeds into feed section 12 through feed line 20. The process fluid then flows through cartridge 16 to process material 2. Eventually the process fluid flows out of cartridge 16 through effluent section 14.
Preferably, process device 10 operates so that cartridge 16 is arranged vertically, as shown in
Turning to
Reinforced wall 22 of cartridge 16 is designed to withstand a clamping force between feed section 12 and effluent section 14, described below. In order to ensure that the process fluid does not leak from processing device 10, cartridge 16 is tightly clamped between feed section 12 and effluent section 14. Wall 22 of cartridge 16 should be rigid enough to withstand the clamping force so that cartridge 16 does not collapse.
Support member 38 is preferably a sintered metal, such as Hastelloy, but can be any material that is permeable to the process fluids flowing through cartridge 16 and that is sufficiently strong to support material 2. Other possible materials of support member 38 include glass, sintered glass, Raney metals, electro-bonded membranes, etched alloy membranes, and fine meshed screens with gaps smaller than the minimum size of material 2, but large enough to allow the process fluid to flow adequately. In one embodiment, cartridge 16 can hold between about 0.1 cm3 to about 10 cm3, and preferably about 3 cm3 to about 5 cm3 of material 2.
The volumes provided above for processing device 10 are not limiting and are provided simply for context in the preferred case of a laboratory-scale device. It is conceivable that processing device 10 can be scaled up to a pilot plant or even a commercial scale or scaled down to micro-scale without varying from the scope of the present invention.
Returning to
In one embodiment, feed section 12 includes a feed channel 40 having an exit end 42 with a generally outwardly extending flange 44 at an exit end 42. Flange 44 encircles a feed port 46 at exit end 42, through which the process fluid flows before passing into cartridge 16. The feed line 20 feeds a process fluid into feed channel 40. Preferably, feed line 20 is made from a flexible material, such as plastic or rubber, to allow for easy movement of feed section 12 while still avoiding breaking or detachment of feed line 20.
Inlet rim 34 of cartridge 16 abuts against flange 44 at exit end 42 of feed section so that inlet rim 34 of cartridge 16 surrounds feed port 46. In one embodiment, feed section 12 includes a seal between feed section 12 and cartridge 16 for sealing between feed port 46 and inlet end 30 of cartridge 16. The seal provides for parallel sealing to effectively seal between cartridge 16 and feed section 12. In one embodiment, shown in
Continuing with
Effluent section 14 provides a path for the process fluid to exit cartridge 16 after the fluid has contacted material 2. Effluent section 14 includes an entrance end 54 having an effluent port 56, an exit 58, and a conduit 60 extending through effluent section 14 between effluent port 56 and exit 58. The process fluid flows out of cartridge 16 and into conduit 60 through effluent port 56, the process fluid can then flow through conduit 60 and out of effluent section 14 through exit 58. An effluent line 62 provides a path for the process fluid to flow away from effluent section 14. Preferably, effluent line 62 is flexible to allow for movement of effluent section 14 while preventing the breaking or detachment of effluent line 62. Like feed section 12, effluent section 14 can also be located either above or below cartridge 16, depending on the desired flow direction of the process fluid.
Continuing with
Outlet rim 36 of cartridge 16 abuts entrance end 54 of effluent section 14 so that cartridge 16 is clamped between effluent section 14 and feed section 12. Outlet rim 36 of cartridge 16 surrounds effluent port 56 so that the process fluid flows into conduit 60. Entrance end 54 may also include an effluent seal for sealing between effluent port 56 of effluent section 14 and outlet end 32 of cartridge 16.
In one embodiment, shown in
As with feed insulating pad 50, effluent insulating pad 66 is preferably made of a thermally resistant and stable material, such as a polymer capable of withstanding the highest expected temperature of processing device 10. Although insulating pads 50 and 66 provide a simple means for sealing and insulating cartridge 16, other seals, such as the embodiment described below, can be used without varying from the scope of the present invention.
In one method, a seal is formed between cartridge inlet end 30 and feed port 46 and between cartridge outlet end 32 and effluent port 56 by clamping cartridge 16 between feed section 12 and effluent section 14. In order to clamp cartridge 16 between feed section 12 and effluent section 14, processing device 10 can include an actuator, such as rack-and-pinion system 112 described below, for raising and lowering either feed section 12 or effluent section 14. In one embodiment, shown in
In a preferred embodiment, shown in
In an alternative embodiment of the present invention, shown in
Insert 70 includes a generally cylindrical main section 74 and a sealing head 76 having a cylindrical outer surface 82 defining a diameter that is larger than the diameter of main section 74. Insert 70 defines an internal conduit 78 running throughout the length of insert 70, wherein the process fluid flows through conduit 78. Sealing head 76 ends in a truncated cone 80 which angles inwardly from outer surface 82 toward feed port 79 at the end of conduit 78. Insert 70 extends through a cylindrical bore 75 defined by the thickness of feed section 12b for translational movement of insert 70 therein. Main section 74 of insert 70 extends above feed section 12b and is engaged by a snap ring 84 which prevents withdrawal of insert 70 from the bottom of feed section 12b. Feed line 20 is connected to insert 70 and feeds the process fluid into conduit 78, as shown in
Sealing head 76 provides a shoulder 86 that retains spring 72 between feed section 12b and sealing head 76 so that spring 72 acts to bias insert 70 away from feed section 12b and toward cartridge 96. A similar, but inverted insert 88 with a spring 90 and a truncated cone 92 is integrated with effluent section 14b to seal between effluent section 14b and cartridge 96 and allow the process fluid to flow from cartridge 96 into conduit 94 and out of effluent section 14b, as shown in
In the alternative embodiment, alternative cartridge 96 differs from cartridge 16 of
When cartridge 96 is placed between effluent section 14b and feed section 12b it is aligned so that frusto-conical sections 98, 99 of cartridge 96 line up with truncated cone 80 of feed section insert 70 and truncated cone 92 of effluent section insert 88. Effluent section 14b or feed section 12b is moved by rack-and-pinion system 112 (shown for moving effluent section 14b in
In the embodiment shown in
Springs 72, 90 provide a force to bias feed section insert 70 tight against frusto-conical section 98 of cartridge 96 and to bias effluent section insert 88 tight against frusto-conical section 99. Springs 72, 90 ensure a tight metal-to-metal seal between inserts 70, 88 and cartridge 96. An advantage of metal-to-metal sealing apparatus 68 is that it can withstand much higher temperatures then traditional elastomer O-ring seals such as VITON™ or TEFLON™.
Returning to
When material 2 has been sufficiently processed, flow of the process fluid is stopped through processing device 10, and gears 114 are rotated so that effluent section 14 is lowered, unclamping cartridge 16 and releasing it from between feed port 46 and effluent port 56. After cartridge 16 is unclamped, cartridge 16 is moved away from cartridge station 18 between feed section 12 and effluent section. A second cartridge can move into cartridge station 18 to repeat the process for a different material 2 or with a different process step.
Preferably, a plurality of cartridges 16 is used with processing device 10 so that a plurality of materials 2 may be screened in a relatively short period of time. Each cartridge 16 of the plurality can contain the same material 2 to be processed, or each cartridge 16 can contain a different material 2 to be processed. Still more preferably, a plurality of cartridges 16 is used in an arrangement allowing automatic and controlled movement of each cartridge 16 into and out of cartridge station 18 of processing device 10.
In order to easily manipulate a plurality of cartridges 16, a cartridge support is used to hold and support the plurality of cartridges 16. The cartridge support can be one of several embodiments for supporting a plurality of cartridges 16. For example, the cartridge support can be a cartridge belt 124 (
Turning to
Preferably, the movement of the cartridge support is automated and computer controlled by a cartridge position controller 130 to allow for automated and rapid performance of processing devices 10 for the processing of materials 2. Several cartridge position controllers 130 for moving cartridges 16 are known in the sample changing art. Cartridge position controller 130 may comprise any mechanical device with a suitably-controlled actuation system to position a selected cartridge 16. Cartridge position controller 130 preferably acts on cartridges 16 to position them in the location of cartridge station 18 and remove cartridges 16 from cartridge station 18. Alternately, cartridge position controller 130 can act on processing device 10 to position cartridge station 18 by locating processing device 10 in alignment with a selected cartridge 16.
Turning to
An alternative arrangement, shown in
A first cartridge 16a can be positioned into cartridge station 18a between first feed port 46a and second feed port 56a of first processing device 10a, where first cartridge 16a is clamped between feed section 12a and effluent section 14a by an actuator to seal cartridge 16a between feed port 46a and effluent port 56a. After first cartridge 16a is clamped and sealed between feed section 12a and effluent section 14a, the first process step is performed on a material 2a in first cartridge 16a. Once the first process step is completed, first cartridge 16a is unclamped from between feed section 12a and effluent section 14a and first cartridge 16a is moved a distance D by cartridge position controller 130 via cartridge belt 124 to cartridge station 18b between feed port 46b and effluent port 56b of second processing device 10b, while a second cartridge 16b is moved into first cartridge station 18a.
Once first cartridge 16a is located in second cartridge station 18b and second cartridge 16b is located in first cartridge station 18a, first cartridge 16a is clamped between feed section 12b and effluent section 14b, and second cartridge 16b is clamped between feed section 12a and effluent section 14a. A second process step is performed on material 2a in first cartridge 16a and the first process step is performed on a material 2b in second cartridge 16b. This process can be repeated for additional process steps at a third processing device 10c, a fourth processing device 10d, etc. The multiple process steps can be performed on material 2a in first cartridge 16a, material 2b in second cartridge 16b, a third material 2c in a third cartridge 16c, a fourth material 2d in a fourth cartridge 16d, etc.
Moving on to
where θ has units of degrees and N is the total number of cartridges holes 148 in carousel. When a first cartridge 16a is desired to be moved out of cartridge station 18 and a second cartridge 16b is desired to be moved into cartridge station 18, carousel 126 is rotated by θ degrees.
Carousel 126 also allows a plurality of processing devices 10a, 10b, 10c that are also arranged in a circular arrangement, as shown in
As shown in
Cartridge tray 128 allows for two dimensional manipulations of cartridges 16 in both the X direction and the Y direction, as shown in
In another embodiment of the present invention, one or more sets 150 of processing devices 10 are provided, wherein each set 150 of processing devices 10 corresponds to all of the cartridges 16 in a particular row of cartridge tray 128. Each set 150 of processing devices 10 performs one or more process steps on materials 2 in the cartridges 16 in a corresponding row. Each processing device 10 of a set 150 can perform the same process step, such as an oxidizing heat treatment step, each processing device 10 can perform a different process step, or banks of more than one processing device 10 can perform different process steps with each processing device 10 in a bank performing the same process step.
The embodiment in
Preferably any apparatus or method of this invention will retain cartridges 16 in a retaining device such as carousel 126, cartridge tray 128, or cartridge belt 124 and rails 132,134 in manner that permits translation movement of the cartridges within the retaining device. This permits the sealing of the cartridge on both ends to occur readily by only applying pressure to one side of the device through movement of only the feed section 12 or outlet section 14 of the processing device 10.
This preference for cartridge movement within the retaining device does not exclude the use of cartridge, retaining device, and processing device arrangements that achieve sealing in a different manner. For example, a fixed cartridge arrangement may rigidly retain cartridges within the retaining device or even have cartridges formed unitarily as part of the retaining device. Such a fixed cartridge arrangements may have enough inherent flexibility for sealing at both ends by the application of movement to only an inlet of section 12 or outlet of section 14. Alternately sealing of the cartridge elements with movement from only one of the inlet or outlet sections may occur by allowing translation of the entire retaining device assembly. In fact, the use of one or more expanding seal elements may obviate the need for any movement of the inlet and outlet sections. Possible arrangements for expanding seals may interpose an expandable element between the seal element and the seal seat of the inlet or outlet section or provide inflation of the seal itself.
Although only three configurations are described above as examples, one having ordinary skill in the art would recognize that any one of several other configurations can be used without varying from the scope of the present invention.
Processing device 10 processes materials 2 using a method that includes the steps of loading material 2 to be processed into a cartridge 16, wherein cartridge 16 includes an inlet, for example at inlet end 30, and an outlet, for example at outlet end 32, positioning cartridge 16 between feed port 46 and effluent port 56, sealing between feed port 46 and cartridge inlet end 30 and between effluent port 56 and cartridge outlet end 32, flowing a fluid through cartridge 16, and releasing cartridge 16 from between feed port 46 and effluent port 56.
Another method includes providing a cartridge support for holding one or more cartridges 16, such as cartridge belt 124, carousel 126 or cartridge tray 128, wherein the positioning step describe above includes moving the cartridge support so that cartridge 16 is positioned between feed port 46 and effluent port 56. The method can also include the steps of clamping the cartridge between feed port 46 and effluent port 56 wherein the sealing step includes the clamping, heating the fluid before flowing the fluid through cartridge 16, and cooling the fluid after flowing the fluid through cartridge 16.
Yet another method includes the steps of removing cartridge 16a from cartridge station 18a, see