• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    The present invention relates to a method for draining a reactor (1) containing a bed of spent catalyst particles (3) and comprising a downwardly inclined drain tube (2) which opens into the reactor (1). This process comprises the following successive steps: a first step consisting in causing the flow of a portion of the catalyst bed (3) out of the reactor via said drain tube (2), and then a second suction step of residue (3 ') of catalyst, carried out by suctioning the catalyst particles remaining in the reactor (1) at the end of the first step by means of a flexible suction sleeve (5) introduced into the reactor via said tube draining device and connected to a suction system (6) located outside the reactor, said sleeve (5) being provided on its outer surface with protuberances and being movable, inside the reactor, in translation and in rotation with respect to said drain tube (2).
    公开号:FR3037823A1
    申请号:FR1555945
    申请日:2015-06-26
    公开日:2016-12-30
    发明作者:Jean Darcissac；Vincent Thevenet；Romain Vial；Lilian Bernard；Pierre Dufresne
    申请人:Europeene de Retraitement de Catalysateurs EURECAT；
    IPC主号:
    专利说明:

    [0001] The present invention relates to a method which allows to completely empty a reactor containing catalyst particles. The process according to the invention is particularly suitable for completely emptying an industrial reactor of spent catalyst particles contained therein. Numerous industrial processes, particularly in the fields of chemistry, petrochemistry and petroleum refining, use solid catalysts in the form of small particles. These catalyst particles are generally arranged in the reactor in the form of one or more superimposed beds (or catalyst layers), each deposited on a support plate. During its use in the reactor, the catalyst is progressively deactivated, and its activity decreases, so that it must be removed from the reactor to be replaced by a new active catalyst. Thus, industrial reactors must be regularly stopped to renew the catalyst bed or beds. This operation takes place in two stages: the emptying of the reactor so as to remove the spent catalyst, then its reloading in active catalyst. These two operations must be performed as efficiently and quickly as possible, so as to minimize the downtime of the reactor, for obvious economic reasons. In addition, the emptying operation must be complete, to completely remove the entire spent catalyst from the reactor. In fact, an incomplete emptying would lead to leaving used catalyst in the reactor, to the detriment of the active catalyst, which would be particularly detrimental to the efficiency of the unit and is in practice not acceptable. However, the complete emptying of an industrial reactor of spent catalyst particles that it contains is a delicate and problematic operation, for various reasons.
    [0002] In the first place, spent catalyst particles tend to be tacky and to agglomerate more or less strongly to each other, which substantially complicates their removal from the reactor.
    [0003] Secondly, the spent catalyst often contains an active phase which can be reactive in contact with air, such as, for example, the active phases containing metal sulfides. Due to the presence of these compounds, the spent catalyst can spontaneously heat up abruptly and significantly, or in some cases self-ignite on contact with air. Most of the corresponding catalysts are classified, according to a United Nations standard, either as self-heating or as pyrophoric. The handling of the spent catalyst is therefore delicate and can be dangerous, and the reactor is usually emptied under an inert atmosphere (usually nitrogen). In order to empty a reactor containing spent catalyst particles, several techniques are known in the prior art: Gravity draining: This is done by opening the lateral drain tube (s) at the bottom of the reactor (or bottom of each catalyst bed for a multi-bed reactor), so as to allow the catalyst to flow out of the reactor under the action of its weight. This allows in the most favorable cases to extract 80 to 85% of the used catalyst contained in the reactor.
    [0004] But the catalyst can also be sticky and poorly flowing or not at all, especially when spent catalyst agglomerates have formed. In this case, it is necessary to use different bed unclogging techniques to engage the flow of the catalyst particles.
    [0005] In all cases, even the most favorable ones, at the end of the gravity-emptying operation, there remains in the reactor a quantity of used catalyst which generally represents from 15 to 20% by weight of the initial catalyst bed, and which typically corresponds to the natural slope angle of this divided solid. This residue of catalyst in the reactor at the end of the gravity drain is commonly called "dig out". Human intervention is then necessary to evacuate the dig out: an operator descends into the reactor and manually removes this residue, for example with a shovel, to the drain tube. This operation presents a particularly important danger: the reactor is under nitrogen, given the self-heating character of the spent catalyst, and regularly fatal accidents occur during these operations. Manufacturers therefore wish today to limit or even completely eliminate such human interventions within the reactors. - Suction emptying: This is usually done from the top of the reactor. The top of the reactor is open, under a nitrogen sweep, the load distributor plate generally present above the bed is disassembled, and the catalytic bed is sucked by means of an industrial vacuum cleaner with nitrogen compensation. The vacuum head is generally guided by an operator to drain the catalyst layer by layer. The solid and the gas are separated via a cyclone. This technique, widely used, has various disadvantages: a high cost; a deterioration of the catalyst particles, sometimes going so far as not to allow the regeneration of the latter for its subsequent use; the presence in the reactor of an operator, at least for the finishing operations, which generates safety problems as described above. Examples of this type of technique are described in US 7,959,870 and WO 2004/058572. Gravity flushing under water: This technique, rather experimental and less commonly used, makes it possible to avoid any human intervention in the reactor under an inert atmosphere. It consists in filling the reactor with water and draining the catalyst / water mixture via the lateral emptying tubes situated at the bottom of the reactor.
    [0006] However, it has major disadvantages: it generates a lot of dirty water, and compromises the possibility of regenerating the used catalyst for reuse. Thus, there has long been a great need for innovative solutions that make it possible to completely, quickly, efficiently and safely empty industrial reactors of spent catalyst particles that they contain. The Applicant has now discovered a new technique for emptying reactors containing spent catalyst particles, which overcomes the disadvantages of the methods of the prior art. The present invention relates to a method for draining a reactor containing at least one bed of used catalyst particles and which comprises at least one emptying tube, which opens into the reactor in the lower part of said bed of particles or below that - this. The method according to the invention comprises the following successive steps: a first step consisting in causing the flow of a portion of the catalyst bed via the said emptying tube out of the reactor, then a second stage of sucking up the residue; of catalyst, by suctioning the catalyst particles remaining in the reactor at the end of the first step by means of a flexible suction sleeve introduced into the reactor via said drain tube and connected to a suction system located outside the reactor, said sleeve being provided on its outer surface with protuberances and being movable in translation and in rotation relative to said drain tube. The method according to the invention makes it possible to empty the reactor of its spent catalyst load in a particularly complete, efficient and rapid manner. The method according to the invention also makes it possible to avoid any human intervention inside the reactor, and makes it possible to improve, in a very important way, the safety of the discharging operations of the spent catalyst. The method according to the invention finally makes it possible to preserve the properties of the spent catalyst and to limit its damage during unloading, which is essential when the catalyst must then be regenerated for later use. The first step of the method according to the invention is to cause the flow of a catalyst bed portion out of the reactor through the drain tube, opening it.
    [0007] This first step is preferably carried out gravityally, i.e. by causing gravity flow out of the reactor of a portion of the catalyst bed via said drain tube. By "gravity flow" is meant that the catalyst flows from the reactor during the first step under the action of its own weight, and is not pushed by mechanical means of thrust inside the reactor (For example, by an operator), or sucked out of the reactor by suction means of the particles. It is typically a conventional gravity flow, such as those known in the prior art.
    [0008] The flow can also be assisted, that is to say that during the first step are implemented means for facilitating the exit of the catalyst from the reactor, for example by means of injection into the reactor. gas reactor under pressure. Moreover, especially in cases where the flow of catalyst does not occur spontaneously during the opening of the drain tube, it is possible, immediately before the first step, to resort to deagglomeration means of the catalyst bed . Such means are known in the prior art. It can act in particular of an injection of gas under pressure (typically, CO2 under pressure).
    [0009] These means make it possible to start the flow of the catalyst particles, after which the catalyst, in the case of a gravity flow, is allowed to flow under the sole action of its weight. Thus, according to one embodiment of the invention, said first step is preceded by a preliminary stage of deagglomeration of the catalyst, which is preferably carried out by injecting into the catalyst bed an inert gas under pressure such as dioxide. carbon or nitrogen. The present invention is applicable to reactors which are provided with at least one emptying tube, which opens into the reactor at or below the bottom of the particle bed. The drain tube can be horizontal, or tilted down. Preferably, it is inclined downwards. In this case, the drain tube preferably has an inclination angle with respect to the vertical ranging from 0 to 75 degrees, more preferably 10 to 60 degrees. During the first step of the process according to the invention a generally substantial part of the used catalyst bed is extracted from the reactor, typically greater than 50% by weight of the initial bed, and in general from 60 to 95% by weight of the initial catalyst bed, more particularly 70 to 90% by weight of the initial catalyst bed. The catalyst residue (or "dig out") is then completely removed from the reactor by means of the second step of the process of the invention.
    [0010] This second step uses a flexible suction sleeve, which is introduced over part of its length into the reactor via the drain tube, once the first step is complete. The end of the sleeve located outside the reactor is connected to a suction device, which makes it possible to suck the remainder of catalyst which enters the sleeve via the end thereof which is introduced into the sleeve. the reactor. Thus, during this second step, the spent catalyst residue is totally sucked in the lower part of the catalyst bed, via the suction sleeve according to the invention.
    [0011] According to the present invention, the sleeve is movable inside the reactor in translation and in rotation with respect to said emptying tube. This means that it can be pushed more or less deeply inside the reactor by thrust means 3037823 7 of the sleeve, and that it can turn on itself thanks to means of rotation of the sleeve . For this purpose, means for guiding the sleeve are advantageously present outside the reactor to enable said sleeve to be moved. Suitable guiding means consist for example of at least two motors that move the sleeve one in translation and the other in rotation relative to the drain tube. The guide means of the sleeve may be attached to the sleeve and / or the reactor by means of a fastening system screwed to the drain tube. These guide means can be controlled manually, automatically or semi-automatically. When the control of the guide means of the sleeve is manual, an operator outside the reactor controls the movements of the sleeve inside the reactor by actuating these guide means. When the control of the guide means of the sleeve is automatic, the guide means are controlled by a computer 20 which executes a program for moving the sleeve inside the reactor. The displacement program can be predefined, that is to say that the movements of the sleeve during the second step have been calculated beforehand, so as to optimize the suction of the "dig out". The shifting program may also be designed to arrange a random shift of the sheath within the reactor. The control of the guide means of the sleeve can also be semi-automatic, that is to say controlled in part via a computer program, and in part by an operator.
    [0012] In addition, according to a particularly advantageous embodiment of the invention, means for detecting the position of the sleeve are present in the reactor. Such means allow to know at any time the exact position of the sleeve in the reactor, and if necessary, optimize its movements.
    [0013] These detection means may comprise a calculation software, which determines progressively the position of the sleeve in the reactor taking into account the movements made (simulation of the position of the device via software compiling the control data. 5 to deduce the position). Other detection means include, for example, radar level detection or ultrasonic level detection systems; systems implementing one or more accelerometers, one or more GPS; vision systems by one or more cameras.
    [0014] According to a preferred embodiment, said detection means comprise one or more camera (s), which makes it possible to display the position of the sleeve in the reactor. Such a camera may for example be positioned on the inner wall of the reactor and / or on the sleeve itself. Various types of cameras can be used for this purpose, including night vision cameras, infrared cameras. Such a camera can also allow if necessary to locate the remaining catalyst, and control accordingly the movements of the suction sleeve.
    [0015] The suction sleeve employed in the present invention is provided on its outer surface with protuberances. These allow the sleeve to hang the surface of the catalyst residue (dig out), and thus to make lateral movements of the sleeve to the surface thereof by causing a simple rotation of the sleeve, 25 is that is to say by turning it on itself: thanks to the protuberances, the sleeve clings to the surface of the catalyst residue, and moves while rolling on it. The protuberances also allow the sleeve to scrape the surface of the catalyst residue and thereby facilitate the stalling of the catalyst and its suction through the end of said sleeve. These protuberances can have very different shapes. They may comprise, for example, and without limitation, grooves, more or less rounded serrations or on the contrary 3037823 9 pointed, bumps, protuberances in the form of strands, spurs, spades, spikes or nails . They can be arranged regularly or irregularly on the outer surface of the suction sleeve. They may be present along the entire length of the suction sleeve introduced into the reactor, or on a part thereof, for example only at the suction head of the sleeve. By "sleeve" means in known manner a hollow conduit. The sleeve according to the invention is flexible, that is to say deformable and particularly capable of deforming in flexion. For this, the suction sleeve is made of a deformable material such as a polymeric material, for example a reinforced polymer, or a flexible metal material. According to a particularly advantageous embodiment, the end of the sleeve introduced into the reactor (that is to say, the suction head of the sleeve) is bent, for example in the form of a "crooked nose". Such a shape makes it possible to facilitate the suction of the catalyst particles to the detriment of the reactor atmosphere. In the case where the reactor comprises several catalyst beds, each bed can be emptied by means of the method according to the invention. This requires the presence on the reactor of at least one emptying tube at the bottom of each catalyst bed. When the spent catalyst to be withdrawn from the reactor is reactive with air, for example when it has a self-heating character, the process according to the present invention is typically carried out by placing and then maintaining the reactor under an inert gas. that is, the catalyst that is removed from the reactor during the two stages of the invention is progressively replaced by an inert gas, such as, for example, nitrogen. This introduction of inert gas into the reactor 30 as it is emptied can be done for example from the top or the bottom of the reactor. The present invention will now be illustrated in more detail and in a nonlimiting manner, with the aid of the appended figures in which: FIG. 1 illustrates the implementation of the first step of the process according to the invention in a reactor industrial production containing a used catalyst bed, FIG. 2 shows the same reactor, at the end of the first stage, FIG. 3 illustrates the implementation of the second stage of the process according to the invention, in the same FIGS. 4 to 7 illustrate examples of protuberances structure that may be present on the surface of the suction sleeve. Figure 1 shows an industrial reactor 1 of the column type, containing a bed 3 of spent catalyst particles. The reactor 1 comprises a downwardly inclined drain tube 2, with an angle of inclination to the vertical of about 45 degrees. The tube 2 opens into the reactor 1 at the bottom of the bed 3 of particles. To enable the first step of the process according to the invention to be carried out, the emptying tube 2 has been opened by opening the drain valve 7, so that the catalyst particles 20 flow out of the reactor 1 through gravitational flow, via the tube 2. The dashed lines 4 show the initial upper level of the catalyst bed 3 before the gravitational flow is triggered, and the arrows in FIG. 1 show the direction of flow of the catalyst. FIG. 2 illustrates the same reactor 1 at the end of the first gravity-emptying step, and shows that, at the end of this stage, there remains in the reactor 1 a residue 3 'of used catalyst which represents here approximately 15% by weight of the initial catalyst bed, and which corresponds to the natural angle of slope of the cluster of catalyst particles. The residue 3 'of catalyst corresponds to the "dig out" which can not be eliminated by simple gravity draining. As illustrated in FIG. 3, according to the second step of the process according to the invention, the residue 3 'of catalyst is then sucked out of the reactor 1 by means of a flexible suction sleeve 5 introduced into the reactor 1 via the drain tube 2.
    [0016] The end of the sleeve 5 introduced into the reactor, that is to say the suction head of the sleeve, is bent. The protrusions present on the surface of the sleeve 5 are not visible on the scale of FIG. 3, but may in particular be as described in FIGS. 4 to 7 below. The sleeve 5 is connected to a suction system 6 located outside the reactor. In addition, the sleeve 5 is movable in translation relative to the axis of symmetry of the emptying tube 2, and rotatable relative to the same axis. For this purpose, a system 10 for driving in translation and in rotation of the sleeve (for example, a pair of motors) is fixed on the flange at the outlet of the emptying tube 2. FIGS. 8. Figure 4a shows an embodiment in which the handle 5 is provided on its outer surface with grooves 9. FIG. 4b shows an embodiment of FIG. cross sectional section of the sleeve 5. FIG. 5 shows an embodiment in which the sleeve 5 is provided on its external surface with a set of crampon-shaped bosses 10, for example regularly arranged on the surface of the sleeve. handle. Figure 6 shows a cross sectional view of the sleeve 5, and illustrates an embodiment in which the handle 5 is provided on its outer surface with serrations 11 having a rounded shape, but which could also be pointed, or a form of hooks. Figure 7 shows an embodiment in which the handle 5 is provided on its outer surface with a set of protuberances 12 in the form of lugs or spikes, regularly arranged on the surface of the sleeve.
    权利要求:
    Claims (13)
    [0001]
    REVENDICATIONS1. Process for draining a reactor (1) containing at least one bed (3) of spent catalyst particles and comprising at least one emptying tube (2), which opens into the reactor (1) in the lower part of said bed (3) of particles or below thereof, the process comprising the following successive steps: a first step of causing the flow of a portion of the catalyst bed (3) out of the reactor via said drain tube (2), then - a second stage of suction of the remainder (3 ') of catalyst, carried out by suctioning the catalyst particles remaining in the reactor (1) at the end of the first stage by means of a flexible suction sleeve ( 5) introduced into the reactor via said drain tube and connected to a suction system (6) located outside the reactor, said sleeve (5) being provided on its outer surface with protuberances and being movable, at the inside the reactor, in translation and in rotation by rappo rt to said drain tube (2).
    [0002]
    2. Method according to claim 1, characterized in that the first step is performed in a gravitational manner, causing the gravity flow out of the reactor of a portion of the bed (3) of catalyst via said drain tube (2).
    [0003]
    3. Method according to any one of the preceding claims, characterized in that during the first step, the portion of the spent catalyst bed (3) extracted from the reactor is greater than 50% by weight of the initial bed, preferably from 60 to 95% by weight of the initial catalyst bed, more preferably from 70 to 90% by weight of the initial catalyst bed.
    [0004]
    4. Method according to any one of the preceding claims, characterized in that during the second step the sleeve (5) is moved by guide means (8) disposed outside the reactor (1). 3037823 13
    [0005]
    5. Method according to the preceding claim, characterized in that the guide means of the sleeve (5) are controlled manually, automatically or semi-automatically.
    [0006]
    6. Method according to any one of the preceding claims, characterized in that means for detecting the position of the sleeve (5) are present in the reactor.
    [0007]
    7. Method according to the preceding claim, characterized in that said detection means comprise one or more camera (s), positioned (s) on the inner wall of the reactor (1) and / or on the sleeve (5).
    [0008]
    8. Method according to any one of the preceding claims, characterized in that the protuberances on the surface of the sleeve (5) comprise grooves (9), serrations (11) more or less rounded or pointed, bumps (10). ), or protuberances 15 in the form of flanges, lugs, spikes (12), spikes or nails.
    [0009]
    9. Method according to any one of the preceding claims, characterized in that the protuberances are present over the entire length of the suction sleeve (5) introduced into the reactor, or a part thereof, for example only at the level of the suction head of the sleeve.
    [0010]
    10. Method according to any one of the preceding claims, characterized in that the end of the sleeve (5) introduced into the reactor is bent.
    [0011]
    11. Method according to any one of the preceding claims, characterized in that the drain tube (2) is horizontal or inclined downwards.
    [0012]
    12. Method according to the preceding claim, characterized in that the drain tube (2) is inclined downwards, with an inclination angle with respect to the vertical preferably ranging from 0 to 75 degrees, more preferably 10 to 60 degrees.
    [0013]
    13. Method according to any one of the preceding claims, characterized in that said first step is preceded by a preliminary step deagglomeration of the catalyst, carried out by injecting into the catalyst bed (3) an inert gas under pressure such than carbon dioxide or nitrogen.
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    同族专利:
    公开号 | 公开日
    TW201707780A|2017-03-01|
    BR102016014948A8|2018-02-27|
    CA2932962A1|2016-12-26|
    CN106268535A|2017-01-04|
    FR3037823B1|2017-08-25|
    JP2021166994A|2021-10-21|
    JP2018051417A|2018-04-05|
    JP6981737B2|2021-12-17|
    KR20170001639A|2017-01-04|
    US10065165B2|2018-09-04|
    US20160375418A1|2016-12-29|
    EP3108959B1|2017-12-20|
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    CN106268535B|2020-12-11|
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    法律状态:
    2016-05-18| PLFP| Fee payment|Year of fee payment: 2 |
    2016-12-30| PLSC| Publication of the preliminary search report|Effective date: 20161230 |
    2017-05-17| PLFP| Fee payment|Year of fee payment: 3 |
    2018-05-16| PLFP| Fee payment|Year of fee payment: 4 |
    2020-03-13| ST| Notification of lapse|Effective date: 20200206 |
    优先权:
    申请号 | 申请日 | 专利标题
    FR1555945A|FR3037823B1|2015-06-26|2015-06-26|METHOD FOR COMPLETELY DRAINING A CATALYTIC REACTOR|FR1555945A| FR3037823B1|2015-06-26|2015-06-26|METHOD FOR COMPLETELY DRAINING A CATALYTIC REACTOR|
    CA2932962A| CA2932962A1|2015-06-26|2016-06-13|Complete drainage process for a catalytic reactor|
    US15/184,562| US10065165B2|2015-06-26|2016-06-16|Method for completely emptying a catalytic reactor|
    DK16175171.4T| DK3108959T3|2015-06-26|2016-06-20|Process for completely emptying a catalytic reactor|
    ES16175171.4T| ES2662896T3|2015-06-26|2016-06-20|Complete emptying procedure of a catalytic reactor|
    EP16175171.4A| EP3108959B1|2015-06-26|2016-06-20|Method for complete draining of a catalytic reactor|
    TW105119795A| TWI748953B|2015-06-26|2016-06-23|Method for completely emptying a catalytic reactor|
    CN201610461616.8A| CN106268535B|2015-06-26|2016-06-23|Method for completely emptying a catalytic reactor|
    SG10201605245UA| SG10201605245UA|2015-06-26|2016-06-24|Method For Completely Emptying A Catalytic Reactor|
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