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WO1997039300A1 - Introduction de matieres inertes pouvant etre fluidisees dans des reacteurs contenant un catalyseur fluidise - Google Patents

Introduction de matieres inertes pouvant etre fluidisees dans des reacteurs contenant un catalyseur fluidise Download PDF

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Publication number
WO1997039300A1
WO1997039300A1 PCT/US1997/002646 US9702646W WO9739300A1 WO 1997039300 A1 WO1997039300 A1 WO 1997039300A1 US 9702646 W US9702646 W US 9702646W WO 9739300 A1 WO9739300 A1 WO 9739300A1
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WIPO (PCT)
Prior art keywords
particles
reactor
particle size
catalyst particles
catalyst
Prior art date
Application number
PCT/US1997/002646
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English (en)
Inventor
Robert E. Trubac
Rudolf A. Overbeek
Original Assignee
Abb Lummus Global Inc.
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 Abb Lummus Global Inc. filed Critical Abb Lummus Global Inc.
Publication of WO1997039300A1 publication Critical patent/WO1997039300A1/fr

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
    • B01J8/24—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles according to "fluidised-bed" technique
    • B01J8/38—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles according to "fluidised-bed" technique with fluidised bed containing a rotatable device or being subject to rotation or to a circulatory movement, i.e. leaving a vessel and subsequently re-entering it
    • B01J8/384—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles according to "fluidised-bed" technique with fluidised bed containing a rotatable device or being subject to rotation or to a circulatory movement, i.e. leaving a vessel and subsequently re-entering it being subject to a circulatory movement only
    • B01J8/388—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles according to "fluidised-bed" technique with fluidised bed containing a rotatable device or being subject to rotation or to a circulatory movement, i.e. leaving a vessel and subsequently re-entering it being subject to a circulatory movement only externally, i.e. the particles leaving the vessel and subsequently re-entering it
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
    • B01J8/24—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles according to "fluidised-bed" technique
    • B01J8/32—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles according to "fluidised-bed" technique with introduction into the fluidised bed of more than one kind of moving particles
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27B—FURNACES, KILNS, OVENS OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B15/00—Fluidised-bed furnaces; Other furnaces using or treating finely-divided materials in dispersion

Definitions

  • the present invention relates to reactors containing fluidized particles, and more particularly to the introduction of fluidizable inert particles into a reactor containing fluidized catalyst particles.
  • Fluidized bed reactors and related systems using fluidized particles are being commonly employed to accomplish various chemical reactions.
  • the reaction is carried out in the presence of a catalyst.
  • the fluidized particles in the reactors comprise, at least in part, fluidizable catalyst particles.
  • One of the factors which has been known to influence the proper hydrodynamics of the fluidized particles is the size distribution of particles in the reactor.
  • To obtain proper fluidization it is necessary to maintain a mixture of fine, medium and large particles.
  • fluidized catalyst especially those where the catalyst particles have the desirable attribute of high resistance to attrition, it has been observed that there is a depletion of fine catalyst particles due to a number of factors.
  • the fine particles that are ultimately removed by a scrubber, and even by a filter are often contaminated such as by sticky material that makes them unsuitable for recycle.
  • This stickiness problem occurs primarily in partial oxidation reactions such as the selective partial oxidation of butane with air to produce maleic anhydride or ammoxidation reactions such as the reaction of propylene with ammonia and air to produce acrylonitrile.
  • the fine catalyst particles which have been cooled somewhat by the time they reach the filter, serve as sites for the condensation of various compounds.
  • VPO vanadium- phosphorous-oxide
  • some of the phosphorous is slowly volatilized from the catalyst and carried out of the reactor to the effluent system where it eventually is condensed and adsorbed onto the fine catalyst particles deposited in the off-gas filter.
  • phosphorous compounds are injected into the reactor. A portion of these compounds is not adsorbed/reacted onto the catalyst in the reactor and contributes further to phosphorous condensation and adso ⁇ tion on the fine catalyst particles in the off-gas filter. The condensation of the phosphorous compounds on the fine particles makes the fine particles sticky when they are recycled back to the reactor.
  • the stickiness and resulting particle agglomeration is a problem particularly encountered in fluid bed partial oxidations, such as the partial oxidation of butane to maleic anhydride and the reaction of propylene with ammonia and air to form acrylonitrile.
  • fluid bed partial oxidations such as the partial oxidation of butane to maleic anhydride and the reaction of propylene with ammonia and air to form acrylonitrile.
  • the prior art teaches the introduction of small inert particles into a poorly fluidizing bed to improve fluidization performance, in such systems as partial oxidation systems with a stickiness problem, the simple introduction of conventional fine inerts is not sufficient and may even have a negative effect.
  • the present invention relates to a method for improving the performance of reactors containing fluidized catalyst particles, and more particularly involves the introduction of materials into the reactor which will tend not only to maintain a desired particle size distribution of the solid particles within a range for proper fluidization hydrodynamics but are of a nature which will improve catalyst performance. Even more particularly, the invention involves the introduction into the reactor of particles of fluidizable "inert" material which have a particle size range selected to produce the desired particle size distribution of the mixed fluidized solids (catalyst plus added inerts) but which also prevent the agglomeration of the catalyst particles present in the reactor.
  • the inert material which is added has a low surface area of less than 1 m 2 /g, more preferably less than 0.75 m 2 /g and most preferably less than 0.5 m 2 /g.
  • the presence of the low surface area inert particles in the reactor has been found to improve the hydrodynamics and reactor performance of catalyst particles which were previously impaired by becoming sticky and/or agglomerated.
  • the inert particles may have a particle size distribution equivalent to that of the catalyst particles or may even be limited to larger particle sizes.
  • the larger inert particles act as heat sinks and dilute the concentration of catalyst particularly in the bottom of the reactor. This tends to distribute the reaction throughout the height of the reactor rather than being concentrated at the bottom.
  • the drawing is a simplified flow scheme illustrating the present invention.
  • reactor 10 contains a bed of particles.
  • This bed of particles normally comprises primarily catalyst particles, but in the present invention it also includes “inert” particles as will be explained and defined hereinafter.
  • a support grid 12 below which is the gas plenum 14.
  • a fluidizing gas supply 16 is introduced into the gas plenum 14 and the gas flows up through the bed of particles at a rate such that the particles in the bed are fluidized.
  • Other designs for introducing and distributing the fluidizing gas can also be utilized, as is known in the art.
  • the materials to be reacted are commonly fed into the reactor 10 at the feed location 18, or can alternatively be included with the gas flow at 16.
  • the gas flow 16 would be primarily air and the feed 18 would be primarily the butane, butylene or benzene.
  • the catalyst would be, for example, a mixed oxide catalyst of vanadium and phosphorous as described in U.S. patents 4,594,433 and 4,653,425.
  • the reactor 10 may be one of a variety of types of fluidized bed reactors such as circulating, turbulent, and bubbling bed reactors.
  • the term fluidized bed reactors also includes dilute phase transport reactors where the solid phase is much less dense and might not ordinarily be considered to be a "bed” as in other fluidized reactor systems.
  • bubbling beds do not elutriate the entire spectrum of solid particle sizes, there is still a carry-over and potential loss of fines.
  • the rate of feed and air flow, as well as the particle size distribution of the catalyst are all coordinated not only for a proper reaction, but also for the particular type of fluidized bed reactor as well known in the art.
  • the gaseous reaction products carrying the elutriated solids exit the reactor 10 overhead at 20.
  • the mixture of reaction products and solids is introduced into a solids separator system 22, such as a typical cyclone separator system, which often consists of several cyclones.
  • the cyclone separator system can be inside the reactor so that separation is accomplished before the gaseous products exit the reactor.
  • the cyclonic action separates the solids from the gas, with the solids leaving through the bottom at 24 and the gas through the top at 26.
  • the separator system is not capable, as a practical matter, even with two or three stages, of removing the finest particles from the gas stream. Merely as an example, particles below about 20 microns are difficult to remove.
  • the circulating solids are essentially all catalyst particles which, for example purposed only, might initially have a particle range from 10 to 60 microns for some types of reactors and perhaps from 10 to 200 microns for other types of reactors. A portion of the smallest particles is not returned to the reactor by the cyclones.
  • the catalyst is subject to attrition and fracture, which produce fines of less than 20 microns.
  • the larger catalyst particles removed at 24 are recycled to the reactor 10 while the finest particles in the gas would be removed at 28 from the product gas 30 by some form of filter 32 (or a scrubber) and then either recycled to the reactor or discarded.
  • Fresh make-up catalyst to replace any lost catalyst is added at 34.
  • fluidizable "inert” particles are added to the reactor at 36 along with the catalyst, or by some other means.
  • the term "inert” in the context of the present invention is defined as particles which are inert with respect to the reactants, the reaction product and the catalyst such that they do not adversely affect or interfere with the basic reaction and catalyst.
  • the inert particles may be reactive with respect to contaminants or by-products in the system or at least adsorb or abrade away such contaminants or by-products.
  • their hydrodynamic benefits result in improving the reactor performance.
  • the inert fluidizable particles which may be employed in the present invention are alumina, silica, titania, magnesia, zirconia, metal carbides, silicon carbide, carbon and zeolites, or mixtures thereof.
  • the inert material should be sufficiently attrition resistant so that it maintains its integrity during the process.
  • the density of the inert particles may be selected to closely match the density of the catalyst particles or the density may be less or even more than that of the catalyst particles. Also, the size range and distribution of the inert particles may match that of the catalyst particles (including fine particles) or it may be adjusted to be different as desired.
  • the catalyst that is introduced into the reactor has fewer fine particles than the optimum for hydrodynamics.
  • the fine particles that are desirable to maintain the proper particle size distribution in the bed and which are not provided as catalyst particles, are instead provided by the inert particles.
  • the particle size distribution of the inert particles would be weighted toward the fine particles and contain a larger proportion of particles below about 45 microns. It can now be seen that all or most of the losses of fine particles, except for attrited or broken catalyst particles, will comprise inexpensive inert particles rather than expensive catalyst.
  • the fine particles which are collected in the off-gas filter 32 need not be recycled to the reactor since they are now inexpensive inerts which can be discarded and replaced by addition to the reactor of fresh inert fine particles.
  • the contaminants on the inert fine particles such as the sticky phosphorous material can be removed by some appropriate process, or if they will not have the same adverse agglomerative and hydrodynamic impacts as catalyst fines when they are recycled, the inert fines can be recycled.
  • the particle size distribution of the inert particles may match that of the catalyst particles (before removal of fine catalyst particles) or even be weighted toward the larger particles.
  • the inert particles, particularly the larger particles act as a heat sink and dilute the concentration of catalyst.
  • the heat/reaction moderation at the bottom can be enhanced, distributing the reaction throughout the height of the bed rather than being concentrated at the bottom as occurs without inerts being present.
  • the inert particles have a low surface area as compared to conventional fines which might have previously been added to fluidized catalyst beds.
  • the inert particles have a BET surface area of less than 1 m 2 /g, more preferably less than 0.75 m 2 /g and most preferably less than 0.5 m 2 /g.
  • BET surface area is the surface area measured by the standard Brunauer, Emmet and Teller technique in square meters per gram).
  • a problem encountered in fluid bed partial oxidations is stickiness and particle agglomeration, resulting in a loss of fluidity.
  • This agglomeration can be caused by a coating on the particle surface due to desired product or byproduct formation, possibly in combination with a migration and concentration of catalyst components on the surface.
  • the loss in fluidity results in poor performance, characterized by lower activity and selectivity, along with difficulty in heat management in these highly exothermic systems.
  • a low surface area inert with a particle size range that is the same as or even larger than the catalyst particle size range, with no particles below 40 microns, will also result in improved fluidization in a "sticky" catalyst bed, accompanied by an increase in activity with no loss in selectivity.
  • alumina-1 with a higher surface area had a negative influence on the selectivity.
  • the specific activity of the catalyst represented by the Frequency Factor (which is a well known measure of the activity of the catalyst), did not increase significantly with alumina-1.
  • the low surface area alumina-2 had a negligible influence on the selectivity while significantly increasing the measured Frequency Factor (2700 vs. 2100).
  • BET surface area inerts does not harm catalyst performance, even in a fixed bed reactor. It may even increase the activity somewhat, because of the larger residence time in the bed. However, dilution with inerts with a larger specific surface area decreased the performance considerably. It is therefore necessary to use an inert which has a very low surface area.
  • the specific activity relative to the catalyst i.e. reaction per weight of catalyst
  • the 75/25 mixture of catalyst and low surface area inerts had 25% higher activity per combined weight of the catalyst plus inerts than the same weight of catalyst by itself.
  • the higher activity can be utilized to perform the reaction at a lower temperature, which may increase selectivity for the desired product, or to increase the feed and product rates of an existing reactor at a given temperature, or to allow some other process changes such as the introduction or increase of a selectivity-enhancement agent which might otherwise be an activity suppressant.
  • Another beneficial feature of adding the inert material can be for the inerts to adsorb contaminants such as the excess phosphorous previously discussed. If the contaminants are adsorbed onto the inert material, they will not be available to form a sticky coating or otherwise contaminate the catalyst.
  • the ⁇ -alumina is active for phosphorous adsorption.
  • Other inert materials for adsorbing potential contaminants are, for example, calcium and magnesium oxides and, in some cases, zirconium and vanadium oxides.
  • the present invention improves the contact of the reactant gases with the catalyst by improving fluidization, decreasing bed density, increasing bed height and increasing the residence time of the reactants in contact with the catalyst in the reactor. It will also reduce the cost of losing fine particles and the amount of catalyst fines generated by attrition or breakage, when fine inerts are utilized in place of fine catalyst. In addition, the use of large or heavy inerts can decrease the adverse impact of localized exothermic reactions at the bottom of the reactor.
  • the inert material which is added, it will vary for each particular situation and will depend upon a variety of factors such as the type and density of the catalyst, the velocity of the gas mixture in the reactor, the need to dilute the catalyst at the bottom, and other relevant factors which all determine the optimum particle size distribution for a specific fluidized catalytic reactor.
  • the inerts have a low surface area.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Combustion & Propulsion (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Dispersion Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • General Engineering & Computer Science (AREA)
  • Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)

Abstract

Une réaction chimique en phase gazeuse est réalisée dans un réacteur à lit fluidisé (10) dans lequel on ajoute une quantité de particules 'inertes' pouvant être fluidisées. Au cours de cette réaction chimique, les particules fluidisées dans le réacteur ont tendance à devenir collante et à s'agglomérer, ce qui a un effet défavorable sur l'hydrodynamique du lit fluidisé et l'efficacité du catalyseur. L'utilisation de particules inertes présentant une petite aire de surface, c'est-à-dire, une surface mesurée selon la technique Brunauer, Emmet et Teller, inférieure à 1m2/g, permet de réduire ou de supprimer ces problèmes. La taille des particules inertes peut se situer dans la place comprise entre la taille des fines, particules qui sont plus petites que les particules de catalyseur, et la taille de particules plus grandes que celles du catalyseur. Dans un mode de réalisation, des fines de catalyseur ne sont pas utilisées, ce qui évite toute perte de fines de catalyseur onéreuses. On obtient une granulométrie de particules appropriée pour assurer une fluidisation correcte et un bon fonctionnement du réacteur en ajoutant des particules inertes, qui comprennent des fines pour remplacer les particules de catalyseurs fines non utilisées. Toute perte de fines due à l'incapacité à les séparer ou due à toute contamination se traduit par une perte de particules inertes non onéreuses et non pas de particules de catalyseur onéreuses. La présence de particules à faible aire de surface permet de supprimer ou d'éviter sensiblement tout effet négatif du caractère collant et/ou de l'agglomération de ces particules sur l'hydrodynamique et les performances de réaction.
PCT/US1997/002646 1996-04-17 1997-02-20 Introduction de matieres inertes pouvant etre fluidisees dans des reacteurs contenant un catalyseur fluidise WO1997039300A1 (fr)

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US63388596A 1996-04-17 1996-04-17
US08/633,885 1996-04-17

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2784602A1 (fr) * 1998-10-20 2000-04-21 Eurecat Europ Retrait Catalys Procede de traitement d'un catalyseur ou d'un adsorbant en lit fluidise
US6403515B1 (en) 1998-10-20 2002-06-11 Institut Francais Du Petrole Process for treating a catalyst or an adsorbent in a fluidized bed
WO2005017073A1 (fr) * 2003-08-05 2005-02-24 Exxonmobil Chemical Patents Inc. Co-alimentation de fines pour le maintien d'hydrodynamique de reacteur efficace
US7145033B2 (en) 2001-12-04 2006-12-05 Bp Chemicals Limited Oxidation process in fluidized bed reactor
US7223896B2 (en) 2004-04-29 2007-05-29 Exxonmobil Chemical Patents Inc. Fines co-feed for maintaining efficient reactor hydrodynamics
US7718811B2 (en) 2002-11-26 2010-05-18 Ineos Europe Limited Oxidation process in fluidised bed reactor
CN103702751A (zh) * 2011-07-12 2014-04-02 阿克马法国公司 在流化床反应器内的连续催化剂再生
WO2020006270A3 (fr) * 2018-06-28 2020-02-06 Ascend Performance Materials Operations Llc Procédés et systèmes d'utilisation de particules de silice dans un réacteur à lit fluidisé

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1305973A (fr) * 1968-12-09 1973-02-07
SU457748A1 (ru) * 1973-06-07 1975-01-25 Московский Ордена Трудового Красного Знамени Институт Стали И Сплавов Способ обжига в кип щем слое мелкозернистых материалов
US4225531A (en) * 1977-03-18 1980-09-30 The Badger Company, Inc. Fluidization promoters

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1305973A (fr) * 1968-12-09 1973-02-07
SU457748A1 (ru) * 1973-06-07 1975-01-25 Московский Ордена Трудового Красного Знамени Институт Стали И Сплавов Способ обжига в кип щем слое мелкозернистых материалов
US4225531A (en) * 1977-03-18 1980-09-30 The Badger Company, Inc. Fluidization promoters

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1002581A1 (fr) * 1998-10-20 2000-05-24 Eurecat Europeenne De Retraitement De Catalyseurs Procédé de traitement d'un catalyseur ou d'un adsorbant en lit fluidise
US6403515B1 (en) 1998-10-20 2002-06-11 Institut Francais Du Petrole Process for treating a catalyst or an adsorbent in a fluidized bed
FR2784602A1 (fr) * 1998-10-20 2000-04-21 Eurecat Europ Retrait Catalys Procede de traitement d'un catalyseur ou d'un adsorbant en lit fluidise
US7145033B2 (en) 2001-12-04 2006-12-05 Bp Chemicals Limited Oxidation process in fluidized bed reactor
US7189871B2 (en) 2001-12-04 2007-03-13 Bp Chemicals Limited Oxidation process in fluidized bed reactor
US7718811B2 (en) 2002-11-26 2010-05-18 Ineos Europe Limited Oxidation process in fluidised bed reactor
WO2005017073A1 (fr) * 2003-08-05 2005-02-24 Exxonmobil Chemical Patents Inc. Co-alimentation de fines pour le maintien d'hydrodynamique de reacteur efficace
EA009187B1 (ru) * 2003-08-05 2007-12-28 Эксонмобил Кемикэл Пейтентс Инк. Совместная подача мелочи для поддержания эффективной гидродинамики в реакторе
US7223896B2 (en) 2004-04-29 2007-05-29 Exxonmobil Chemical Patents Inc. Fines co-feed for maintaining efficient reactor hydrodynamics
CN103702751A (zh) * 2011-07-12 2014-04-02 阿克马法国公司 在流化床反应器内的连续催化剂再生
WO2020006270A3 (fr) * 2018-06-28 2020-02-06 Ascend Performance Materials Operations Llc Procédés et systèmes d'utilisation de particules de silice dans un réacteur à lit fluidisé
US11059774B2 (en) 2018-06-28 2021-07-13 Ascend Performance Materials Operations Llc Processes and systems for using silica particles in fluid bed reactor
US11680038B2 (en) 2018-06-28 2023-06-20 Ascend Performance Materials Operations Llc Processes and systems for using silica particles in fluid bed reactor

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