WO2001027607A1 - Sondes in-situ pour processus - Google Patents

Sondes in-situ pour processus Download PDF

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Publication number
WO2001027607A1
WO2001027607A1 PCT/US2000/027693 US0027693W WO0127607A1 WO 2001027607 A1 WO2001027607 A1 WO 2001027607A1 US 0027693 W US0027693 W US 0027693W WO 0127607 A1 WO0127607 A1 WO 0127607A1
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WO
WIPO (PCT)
Prior art keywords
reactor
test material
catalyst
rod
end portion
Prior art date
Application number
PCT/US2000/027693
Other languages
English (en)
Inventor
Donald A. Szczepanski
Mark Bergeron
Original Assignee
Huntsman Petrochemical Corporation
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Huntsman Petrochemical Corporation filed Critical Huntsman Petrochemical Corporation
Priority to AU78691/00A priority Critical patent/AU7869100A/en
Publication of WO2001027607A1 publication Critical patent/WO2001027607A1/fr

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Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N17/00Investigating resistance of materials to the weather, to corrosion, or to light
    • G01N17/002Test chambers
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N17/00Investigating resistance of materials to the weather, to corrosion, or to light

Definitions

  • the present invention relates to a combination of wares which comprise a system for evaluating a material which may include catalysts, sorbents, adsorbents, molecular sieves, and other heterogeneous test materials under actual process conditions.
  • a material which may include catalysts, sorbents, adsorbents, molecular sieves, and other heterogeneous test materials under actual process conditions.
  • the present invention is directed at a method for exposing a solid substance to a chemical process stream during the normal flow of a process stream, while maintaining the flow of the process stream uninterrupted by acts or steps associated with the exposure of the solid substance to the process stream.
  • a solid substance may be placed within the plumbing, pipes, fixtures, or hardware ("process wares") in the location where the process stream normally exists, prior to causing the process stream to exist in the process wares, such as in the case immediately prior to the start-up of a reactor system.
  • a solid substance may be introduced into the process stream while the process is live, from outside of the process wares in which the process stream is contained, without any leakage of the contents of the process stream to the surroundings of the container, and without any leakage of the contents of the surroundings into the process stream.
  • the invention also comprises means for removal of the solid substance from the process stream. Further, the invention comprises means for altering the location of the solid substance within the process stream.
  • the invention also includes the analysis of the solid substance either before or after (or both) exposure to the process stream. According to the invention, the insertion and removal of a sample of solid substance, such as a catalyst test sample, desiccant, or other desired sorbent may be accomplished within any chemical process line, storage vessel, reaction vessel, or any other containment device or system, while maintaining the process flow and/or conditions for evaluation of the effect of processing conditions on the sample, without the need to shut down or otherwise substantially alter the normal operation of the particular process.
  • a sample of solid substance such as a catalyst test sample, desiccant, or other desired sorbent
  • test materials include without limitation candidate catalyst materials ("test materials"), by permitting one to insert or remove test materials from a commercial reactor or process stream during its normal operation.
  • Test materials suitable to be inserted or removed from a reactor according to the invention include by way of illustration only and not by any means delimitive: desiccants, acid indicators, base indicators, adsorbents, corrosion indicators, and catalyst materials.
  • desiccants include by way of illustration only and not by any means delimitive: desiccants, acid indicators, base indicators, adsorbents, corrosion indicators, and catalyst materials.
  • containing means (as herein defined) and inserted or isolated from the reactor according to the invention is a suitable material useful for evaluation of reactor performance or performance of the solid substance according to the invention.
  • a chemical reactor In association with a combination and process according to the present invention in its intended function, there must also be present a chemical reactor, vessel, process stream, etc., and such is conveniently provided by most closed-loop chemical reactor systems. These typically include a feed line, a return line, and a reactor, although other reactor systems and process streams are suitable for use in accordance with the process and wares of the instant invention provided they contain one or more gaseous or liquid reactant(s).
  • the invention also includes a valve means attached to a reactor, wherein the valve means is adapted to receive the containing means according to the invention, wherein the valve means provides for isolation of conditions outside of the reactor from those conditions inside the reactor during insertion of the containing means into the reactor, or during removal of the containing means from the reactor, or during reactor operation when the containing means is in a stationary position within the feed line.
  • an exposed test material may be analyzed for a number of physical and/or chemical properties, depending upon the nature of the test material and the purpose of the evaluation. For example, when the test material is a catalyst, some possible analyses to be carried out are those relating to the presence of catalyst poisons, catalyst durability, activity, selectivity, etc.
  • FIG. 1 is a schematic diagram of a process vessel having a feed line and a return line;
  • FIG. 2 is a schematic view of a block valve equipped with wares according to the invention
  • FIG. 3A is a side schematic view of the wares associated with one form of the present invention.
  • FIG. 3B is a side schematic view of the wares associated with one form of the present invention
  • FIG. 3C is a side schematic view of the wares associated with one form of the present invention
  • FIG. 4A is a perspective view of a containing means according to one form of the invention.
  • FIG. 4B is an end perspective view of a containing means according to the invention. Detailed Description
  • test material is a catalyst. While illustration of the invention is served well by this description, the process and hardwares associated herewith should not be considered to be in any way limited by such mention.
  • the combinations and processes provided according to the invention are suitable for use with any system in which a bed of heterogeneous particles bring about any compositional or physical change, whether they be considered as reaction vessels, pipelines, kettles, autoclaves, furnaces, crackers, distillation apparati adsorption, absorption, etc.
  • one preferred form of the invention includes the loading of the containing means described below with a catalyst material, it is within the scope of the invention to load other materials, which may comprise any solid matter (including particulate matter) into the containing means, including without limitation: acid or base indicators, adsorbents, absorbents, desiccants, filter media, zeolites, corrosion indicators, activated charcoals, scavengers, etc.
  • FIG. 1 there is shown a general schematic representation of a reaction vessel 2, to which is connected at least one feed line 4, and a return line 6.
  • the feed line and return lines are connected to a pre-heat exchanger 8, the use of which is well known to those skilled in the art of heterogeneously catalyzed reactions.
  • a block valve or process nozzle 10 in line with the feed line 4 is a block valve or process nozzle 10, and such are well known in the art of chemical processing equipment.
  • FIG. 2 shows a more close up view of the block valve or process nozzle 10 and its relation to other portions of feed line 4, with a device adapted to carry out a process set forth herein in position at a suitable and desired process location.
  • One preferred combination adapted to carry out the process of this invention includes a rod portion 20 having a first and second end portion that an operator may use to alter the position of the containing means 12 disposed on the second end portion by movement of the first end portion of the rod, by hand or with the aid of other machinery.
  • containing means includes any container having any configuration into which solid particles of any material to be tested may be placed.
  • Such term includes such containers having any geometrical shape, including without limitation spherical, rectangular solid, square solid, cylindrical, etc., and which also includes at least one opening in one of the faces or outer surface of its construction so as to permit the process stream present (which in one embodiment may be one or more gases) to pass through the walls of the container and contact the matter housed in the containing means, which may be a catalyst in one form of the invention.
  • a preferred containing means according to the invention includes a plurality of holes on its faces or outer surface, wherein the holes are smaller than the size of the particles which are to be contained in the containing means.
  • a wire mesh, inert bag, or polymeric netting may be used to contain the heterogeneous particles, and then the mesh, wire, or netting is inserted into the containing means, in which embodiment the containing means has larger holes in its outer surface or wall than would otherwise have been possible in the absence of such mesh, wire, or netting.
  • Typical materials of construction for the frame portion of containing means into which catalysts are to be contained are stainless steels or other metallurgies as may be appropriate for the process under review, although any material which is inert to the reactant(s) encountered may be utilized as a material of construction.
  • FIG. 2 are also shown rod collar 14, bleeder valve 16 (which may be considered a vent), packed compression fitting 18, which is also often referred to as a "bladder valve” or “packing gland” by those skilled in the art, first end portion 24 of rod 20, and flange 22.
  • the containing means may be inserted into a reactor or a process line associated therewith by first connecting the packing gland mounting flange 22 to the closed block valve or process nozzle 10, closing vent valve 16, opening block valve or process nozzle 10, and then passing the basket through the opened block valve or process nozzle 10 by means of the rod 20 through the packing gland 18.
  • the packing gland 18 provides a seal through which the rod can be moved to position the containing means in the process stream, while maintaining the contents of the reactor in isolation from the surroundings.
  • the containing means Prior to the above insertion procedure, the containing means is first charged with the desired test material. The charged containing means 12 and associated rod 20 are then placed in the mounting flanged packing gland 18. Next, the flanged packing gland holding the charged containing means is mounted to the process block valve or process nozzle 10. Then, once the flanged packing gland 18 is attached to the process block valve or process nozzle 10, the block valve or process nozzle valve is opened and the packing gland is loosened just enough to allow the rod to slide through the packing gland and move the containing means into the process.
  • FIG. 3A shows the wares associated with the aforesaid process in accordance with a preferred form of the invention.
  • process stream 19 contained in a reaction vessel, reactor, pipe, etc., which is isolated from the ambient conditions.
  • a block valve or process nozzle 10 and associated flange 7 by which the contents of the reaction vessel are accessible.
  • An element of the wares of the invention is the combination comprising a flange 13 which is complementary to flange 7, and which includes a tubular portion 69 having a first end portion that is connected to said flange 13 and a second end portion that has packed gland 73 (packed compression fitting) affixed to it.
  • the packed gland portion 73 includes a seal disposed in an effective position to extend coextensively about the rod 20 to substantially preclude any exchange of matter from one side of the seal to the other, and particularly to isolate the ambient conditions from the process stream 19 when a process according to this invention is carried out.
  • the containing means 12, rod portion 20 is also shown in FIG. 3A.
  • FIG. 3B shows the wares according to FIG. 3A; however having the flanges 13 and 7 mated to one another by conventional means, such as bolts 30.
  • the valve 10 is closed, thus maintaining the process stream separate from the containing means 12.
  • valve 10 is opened and the rod portion 20 is caused to be moved so as to expose containing means (and its contents) to the process stream 19, as such configuration is more clearly shown in FIG. 3C.
  • rod portion 20 may be withdrawn and valve 10 subsequently closed.
  • Pressure is equalized with ambient pressure in space 88 surrounding the containing means by opening the bleeder valve 16. After pressure equalization, the containing means is removed by disconnecting the flanges 13 and 7 from one another to recover the contents of the containing means for subsequent study or analysis.
  • FIG. 4A is a perspective view of a containing means 12 according to a preferred form of the invention, in which the containing means includes a first collar-shaped end portion 103 and a second collar shaped end portion 105, which end portions are connected to one another by means of a plurality of support rods 101, thus providing spaces 131 inherent in the construction as a whole.
  • the spaces 131 between the support rods 101 are covered by a perforated metal sheet or metal screen to contain the test material.
  • the inner portion 107 of the second end portion 105 is provided with threads which are complementary to those on plug portion 109, which may be conveniently affixed to the end of the containing means once a desired material has been charged to the containing means, by twisting.
  • the first collar shaped end portion includes a bottom portion 169 comprising threads 111 which are complementary to threads 113 that are disposed on the end of rod 20, to provide convenient attachment/disengagement of the rod portion 20 from the containing means 12.
  • a provision 181 for a locking set screw having a bore that is generally perpendicular to the axis of the threads 111 is preferred, but not necessary.
  • FIG. 4B is a side view of the containing means, showing the locations of the support rods 101 according to one preferred form of the invention.
  • the wares associated with carrying out a process comprises: a) a rod portion having a first and second end portion, b) a means for containing a solid material ("containing means"), wherein the containing means is attached to the second end portion of the rod portion to form a rod/containing means composite; and 3) a tubular portion having a first end portion and a second end portion, with a packing gland disposed on said first end portion, wherein said packing gland includes a hole disposed through it that is adapted to receive a rod and to maintain such rod to be slidably mounted within such hole, and further including a seal which extends coextensively about said rod and said packing gland hole to effectively preclude contact of matter on one side of the end cap with matter on the other side of said end cap.
  • containers that are functionally capable of containing a test material while permitting conditions encountered in a reactor to penetrate its walls (including chemical composition, temperature, and pressure) into it to contact a test material contained in it are indicated as being useful according to the invention, including without limitation, french-fryer baskets, covered colanders, cylindrically shaped constructions having mesh walls, and the like.
  • the main criteria is that the container must possess walls which contain a plurality of pores that are smaller in size than the test material so as to prevent the test material from exiting the containing means.
  • a containing means may include a container having a pore larger than the size of the test material, provided an auxiliary containing means is used.
  • an alternative form of the invention comprises the placement of catalyst spheroids having a 5 mm diameter into a nylon mesh bag having a pore diameter of 3 mm, and then placing the whole bag into a containing means such as that depicted in FIG. 4, having pores obviously larger than the individual catalyst particles.
  • the words "containing means are intended to be understood as including the nylon mesh bag utilized, or a functional equivalent thereof, regardless of its materials of construction.
  • reactor includes a reactor system which may in the case of a batch process include an open or closed reactor pot or kettle, and any pipes, lines, recirculating loops, and other conduits connected to such pot or kettle which are caused to contain a static or moving reactant or other material present during the normal operation of the reactor. These include solvents, raw materials, intermediate products, finished products, coolants, lubricants, and the like.
  • a continuous process In the case of a continuous process, it is true that often there exists in association with such continuous process a main reactor pot or kettle, and various pipes, lines, recirculating loops, and other conduits connected to the pot or kettle which are caused to contain a static or moving reactant or other material present during the normal operation of the reactor. Often, a continuous process includes an inlet stream which is caused to pass into the reactor and undergoes a chemical reaction to form the desired product and some undesired side-reaction products.
  • a stream of material containing the desired product and side-reaction products to be drawn off from the reactor at a selected rate, and fed through a transmission pipe to a second processing unit that is in fluid contact with the reactor (which may be a scrubber, refining unit, heat exchanger, or other process equipment, and which may carry out various functions, including separation of the desired product and other materials which may have a deleterious effect on the performance of the reactor).
  • a second processing unit which may be a scrubber, refining unit, heat exchanger, or other process equipment, and which may carry out various functions, including separation of the desired product and other materials which may have a deleterious effect on the performance of the reactor.
  • a return line to send the stream back to the reaction vessel, pot, or kettle from the processing unit.
  • the word “reactor” includes the transmission pipe(s), the return line(s), any second processing unit(s), and any other piece of process equipment that is in fluid contact with the contents of the reaction vessel, pot, or kettle, since it is possible to carry out the process of this invention utilizing the system herein described wherein the hardwares of the system of this invention may be connected to any of the aforesaid portions of the reactor systems described.
  • the "reactor” is intended to include all plumbing, fixtures, pipes, wares, tubes, reaction vessels, etc. that are in fluid contact with the region where the main intended chemical reaction or physical change occurs.
  • the reaction vessel is merely a tube, as in cases of “tubular reactors” or “ shell and tube heat exchangers " as such are commonly referred to in the art.
  • Systems which include tubular reactors or shell and tube heat exchangers also include feed lines leading to the reactor and transmission lines leading out of the reactor and to other pieces of process equipment which are in fluid contact with the contents of the reactor.
  • the wares of the system of the invention may also be located on a parallel loop as illustrated in Flow Diagram I:
  • Flow Diagram I there is a zone where the intended reaction or physical change occurs (the reaction zone), which has a recycle loop A flowing from the exit portion of the reaction zone back into the inlet portion of the reaction zone, where reactants are normally caused to enter.
  • the exact location where one locates the wares of the system of the instant invention in order to carry out the process of the invention is not critical, but rather may be selected by the user depending upon the particular goals of the evaluation to be carried out.
  • the test material In cases where a set up according to Flow Diagram I is employed, it is possible for the test material to be contained within a section of pipe, containing means, or the like located at position X.
  • Insertion of the test material into the reactor then entails opening either or both of valves Bl and B2 prior to or after the time when the valve in recycle loop A is opened during normal process operation. Isolating the test material may be readily accomplished by closing the valves Bl and B2. Once Bl and B2 are closed, then the test material may be removed from the reactor wares entirely, and subjected to any selected chemical analysis. It is most preferable, however, that when the test material used to monitor a chemical process in accordance with the invention is a catalyst material, the test material is located within either the feed line to the reactor, or, when a heated zone is needed that is only available within the reactor, the test material is preferably located within the reactor.
  • a reactor which contains a catalyst charge when it is operated under normal operating conditions will contain a known amount of catalyst, the exact quantity and configuration of which is typically determined by engineers having a good reactor economics background and historical information on which to base the desired amount of catalyst.
  • a quantity of catalyst is known as the "normal catalyst charge" for such a reactor.
  • the containing means is preferably of such capacity that the total amount of test material (catalyst) that is inserted into the reactor according to this invention using a containing means is less than 10.0 % of the normal catalyst charge for the reactor.
  • the amount is between 10.0 % and 5.0 %, including every hundredth percentage therebetween, more preferably still the amount is between 5.0 % and 0.50 %, including every hundredth percentage therebetween, and most preferably the amount is 0.50 % and 0.001 % of the total catalyst charge.
  • the total mass of the test material is between 10 grams and 2500 grams, with 1000 grams being preferred because of its representative size and ease in handling (insertion, isolation).
  • the exact mass of the test material used is not critical, provided that the user is able to derive meaningful results from the test material by analysis, either chemical or by observation or some other method.
  • catalytic substance means any substance that is capable of existing in a solid form which behaves as a catalyst in accordance with the definition of a catalyst accepted by chemists everywhere, namely that the substance must be capable of increasing the rate of reaction of one chemical species with itself, or between two or more reactants, without undergoing any chemical change itself, regardless of whether the catalytic activity of the substance is derived from its reducing an energy of activation (Ea) of a reaction, by providing an alternative kinetic route, or by any other means.
  • Ea energy of activation
  • the rod/containing means combination described earlier contains a provision for adjusting the location of the containing means within the reactor.
  • This is an advantage of the invention, because by placing a test material in different locations within a reactor it is possible to determine the exact conditions which exist at a particular location, which conditions may differ from those conditions at other locations. Such information is important, because it would enable the user to identify places where potential "hot spots" or discontinuities in flow might occur, or to identify irregularities in flow, which information can then be subsequently used in reactor modification towards increasing the overall performance of the reactor.
  • a containing means attached to the end of a rod other means for adjusting or altering in a controllable fashion the location of the containing means may be utilized in accordance with the invention, provided they are functionally equivalent.
  • suitable means include the use of a magnetically susceptible material (such as iron, cobalt, nickel or their alloys)attached to, or as an integral part of the containing means, in conjunction with a magnet or solenoid located externally to the reactor.
  • the rod portion described herein may contain threads along its shaft, and there may be included a complementary female thread portion located on the shaft, which threaded portion functions as a sealing means when inserted into a pipe as set forth earlier herein.
  • the rod described earlier may be stricken with graduations along its length, which are marked in such a way that a user of the invention may know the location of the containing means within the reactor.
  • Other means for causing movement of a container within a reactor which are known to those skilled in the art may be used in this invention as a means for adjusting the location of the containing means. Through such means the location of the containing means within the reactor may be adjusted.

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  • General Physics & Mathematics (AREA)
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Abstract

L'invention concerne un système et un procédé permettant d'introduire et de retirer des matériaux au cours d'un processus, lorsque ce processus suit un déroulement normal, ou un autre déroulement répondant à des conditions définies, y compris des conditions qui ne sont pas ordinairement considérées comme utiles pour le matériau solide sélectionné. Grâce à ce système et à ce procédé un nombre important d'informations relatives à ces matériaux peut être obtenu et évalué. Ces matériaux peuvent être des solides d'essai hétérogènes et peuvent comprendre des catalyseurs, des dessicatifs, des indicateurs etc.
PCT/US2000/027693 1999-10-08 2000-10-06 Sondes in-situ pour processus WO2001027607A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AU78691/00A AU7869100A (en) 1999-10-08 2000-10-06 In-situ process probes

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
US15830099P 1999-10-08 1999-10-08
US60/158,300 1999-10-08
US16165899P 1999-10-21 1999-10-21
US60/161,658 1999-10-21

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WO2001027607A1 true WO2001027607A1 (fr) 2001-04-19

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2021108412A1 (fr) * 2019-11-25 2021-06-03 Saudi Arabian Oil Company Procédé de test de catalyseur dans des réacteurs à lit fluidisé utilisant des capsules de catalyseur

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US3487695A (en) * 1968-06-12 1970-01-06 Chevron Res Gas lift catalyst sampler
US3787183A (en) * 1972-02-09 1974-01-22 Catalyst Services Inc Method of analyzing catalyst action
DE2619363A1 (de) * 1975-04-30 1976-11-04 Paul Kiehn Apparat zur automatischen erzeugung von gasen (wasserstoff-, sauerstoff-, chlorgasen usw.) unter aufladung eines festen stoffes (katalysator oder dergleichen) metalle, salze usw. in einer unter druck stehenden fluessigen loesung, ohne unterbrechung der laufenden reaktion
US4071324A (en) * 1976-06-01 1978-01-31 Luther James Reid Chemical reactor
DD132279A1 (de) * 1977-05-09 1978-09-13 Jochen Nelles Reaktor zur untersuchung chemischer reaktionen
DE2938343A1 (de) * 1978-09-21 1980-04-10 Salonen Ari Heimo Kalevi M Sc Probenfoerdervorrichtung
US4421723A (en) * 1982-07-20 1983-12-20 Chevron Research Company Method and apparatus for supporting radial reactor centerpipes to accommodate thermal cycling
US4726935A (en) * 1984-11-12 1988-02-23 Babcock-Hitachi Kabushiki Kaisha Apparatus for removing nitrogen oxides
US4958527A (en) * 1989-06-14 1990-09-25 The Dow Chemical Company Sample valve assembly for on-line sampling of granular materials

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Publication number Priority date Publication date Assignee Title
US3487695A (en) * 1968-06-12 1970-01-06 Chevron Res Gas lift catalyst sampler
US3787183A (en) * 1972-02-09 1974-01-22 Catalyst Services Inc Method of analyzing catalyst action
DE2619363A1 (de) * 1975-04-30 1976-11-04 Paul Kiehn Apparat zur automatischen erzeugung von gasen (wasserstoff-, sauerstoff-, chlorgasen usw.) unter aufladung eines festen stoffes (katalysator oder dergleichen) metalle, salze usw. in einer unter druck stehenden fluessigen loesung, ohne unterbrechung der laufenden reaktion
US4071324A (en) * 1976-06-01 1978-01-31 Luther James Reid Chemical reactor
DD132279A1 (de) * 1977-05-09 1978-09-13 Jochen Nelles Reaktor zur untersuchung chemischer reaktionen
DE2938343A1 (de) * 1978-09-21 1980-04-10 Salonen Ari Heimo Kalevi M Sc Probenfoerdervorrichtung
US4421723A (en) * 1982-07-20 1983-12-20 Chevron Research Company Method and apparatus for supporting radial reactor centerpipes to accommodate thermal cycling
US4726935A (en) * 1984-11-12 1988-02-23 Babcock-Hitachi Kabushiki Kaisha Apparatus for removing nitrogen oxides
US4958527A (en) * 1989-06-14 1990-09-25 The Dow Chemical Company Sample valve assembly for on-line sampling of granular materials

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Title
W.A. SMIGIEL ET AL.: "Development of a microreactor system to measure catalytic activity on ion-implanted, monocrystalline supports", INDUSTRIAL & ENGINEERING CHEMISTRY FUNDAMENTALS, vol. 18, no. 4, November 1979 (1979-11-01), pages 419 - 422, XP002937630 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2021108412A1 (fr) * 2019-11-25 2021-06-03 Saudi Arabian Oil Company Procédé de test de catalyseur dans des réacteurs à lit fluidisé utilisant des capsules de catalyseur

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