A solid particle sampling device having at least one capacitive valve

Abstract

The present invention relates to a device (10) for sampling solid particles from a sealed chamber (12), the sampling device (10) comprising a tubular body (18) having a sampling head (16), the sampling head (16) being configured to sample a volume of solid particles (14) from the chamber under the influence of gravity, the device comprising a tubular duct (52) attached to the tubular body (18) and forming a non-zero angle with the tubular body (18), the tubular body (18) comprising a deflector (50) for deflecting the solid particles (14) into the tubular duct (52). Further, the sampling device (10) comprises a capacitive valve for removing the solid particles, the valve being arranged downstream of the tubular duct (52). The present invention also relates to a method for sampling solid particles and a method for upgrading the sampling device (10).

Description

Technical Field

[0001] The present invention relates to the field of solid particle sampling from sealed enclosures such as silos, hoppers, reactors, regenerators or adsorbers.

[0002] More particularly, the present invention relates to a sampling device that enables the gravity sampling of solid particles in the form of granules, extrudates, balls, such as those used for example in catalysts or adsorbents.

[0003] When solids divided into particles are fed into an enclosure operating under pressure and / or at high temperature, or when they are placed or transported by gravity in an enclosure in which they are stored, it is often necessary to take a sample of the solid.

[0004] The main purpose of this sampling is to check the mechanical or physico-chemical properties of the solid particles and thus to detect impurities that may have settled on their surface, or to monitor the evolution of the quality of the solid being stored or in transit.

[0005] Thereby, in particular, it becomes possible to understand the reasons for possible failures, to check the storage behavior of solid particles over time or to predict the maximum operating time of solid particles, and thus to correct or predict possible problems.

[0006] In the case of a purification plant using solid particles, it may also facilitate the monitoring of units including for example a catalytic reactor, and thus it may be possible to optimize its operation.

Background Art

[0007] To sample solids from an enclosure, Patent Document 1 discloses, inter alia, a sampling device that enables sampling of a solid material from a sealed enclosure, for example, a reactor that enables catalytic cracking of hydrocarbons in the presence of a catalyst.

[0008] As described in more detail in this document, sampling is carried out using a sampling head that is fed into the enclosure and carried by the body of the device. This sampling head includes a receptacle with a recess at the top and a protrusion at the bottom, and two slotted rotating disks that are rotationally driven by a shaft controlled by any known means. During the first rotation of these disks, the solid sample can enter the receptacle through an upper recess controlled by one of the disks, while the other disk seals the recess at the bottom. After another rotation of these disks, the upper recess is sealed by one of the disks, while the other disk empties the recess at the bottom to allow the solid sample to be sent to a pipe.

[0009] Patent Document 2 (Patent Document 3) also relates to a solid particle sampling device. In this patent application, the solid particles collected through the sampling head are fed through a pipe to the inlet of a first valve. The opening of the first valve allows the solid particles to be fed into an airlock. A bleed valve connected to the airlock enables purging of the airlock. The first valve thus remains closed, the bleed valve is opened, and then closed after the purging is complete. Finally, another valve connected to the airlock can discharge the solid particles contained in the airlock.

[0010] The valves used are typically conical ball valves, spherical ball valves, or parallel slide gate valves with a replacement ring.

[0011] However, sampling devices using these valves have several drawbacks.

[0012] The valves wear out early. In fact, when solid particles are sampled from the enclosure, they are stored inside the device's body and then, under the influence of gravity, are stored in the direction of the solid particle flow at the upstream and downstream valve inlets from the airlock and then recovered into the outer container. The solid particles sampled from the enclosure are generally at a high temperature (according to the application, for example, 150 °C to 550 °C). They are therefore stored at the valve inlets at a high temperature.

[0013] While the valve is gradually opening, the solid particles rub against the surface of the ball moving for the opening at a high temperature. Then, the solid particles can flow into the airlock or the outer container through the open valve under gravity. This friction of the solid particles against the surface of the ball causes erosive wear of the ball and / or the valve, and the ball / sheet contact provides the sealing of the valve. This wear requires regular replacement of the ball and / or the sheet, or the entire valve, which results in additional operating costs.

[0014] In addition, this wear may cause leakage of the fluid contained in the enclosure, especially when the fluid is a gas, and it is more difficult to provide airtightness than liquid tightness. These leaks may also cause the decompression of the enclosure when it is under pressure.

[0015] To overcome such wear, known solutions consist of using surface treatments on the balls and / or sheets of non-capacitive valves used to increase the wear resistance of these components.

[0016] Furthermore, the valves used are more sensitive to errors in valve handling or sequence. In fact, bad sequence or handling errors can cause the fluid (especially gas) to escape from the enclosure, which can also cause its decompression when the enclosure is under pressure.

[0017] The present invention aims to overcome the above-mentioned drawbacks by means of a solid particle sampling device using at least one capacitive valve.

Prior Art Documents

Patent Documents

[0018]

Patent Document 1

Patent Document 2

Patent Document 3

Summary of the Invention

Means for Solving the Problems

[0019] (Summary of the Invention) The present invention relates to a device for sampling solid particles from a sealed enclosure. The sampling device comprises a tubular body carrying a sampling head, the sampling head being configured for gravity sampling of a predetermined volume of solid particles from the sealed enclosure. The sampling device comprises a tubular pipe attached to the tubular body and forming a non-zero angle with respect to the tubular body. The tubular body comprises a deflector for deflecting solid particles within the tubular pipe. In addition, the sampling device comprises a first capacitive valve for discharging solid particles, the first capacitive valve being arranged downstream from the tubular pipe in the flow direction of the solid particles within the sampling device.

[0020] Preferably, the volume of the capacitance of the first capacitive valve is larger than the predetermined volume, and the volume of the capacitance of the first capacitive valve is preferably at least 1.05 times, more preferably at least 1.15 times the predetermined volume.

[0021] Advantageously, the first capacitive valve comprises a single sheet and a capacitive ball, and this single sheet is upstream of the capacitive ball.

[0022] Alternatively, the first capacitive valve comprises a first sheet, a second sheet, and a capacitive ball, the first sheet is upstream of the capacitive ball, and the second sheet is downstream of the capacitive ball.

[0023] Advantageously, the first capacitive valve is selected from a capacitive spherical valve, a capacitive conical ball valve, or a capacitive cylindrical ball valve.

[0024] According to a modification of the present invention, the sampling device comprises a second valve downstream of a tubular pipe for the release of solid particles, the second valve is upstream or downstream of the first capacitive valve, and the first capacitive valve and the second valve are connected to each other directly or by an airlock.

[0025] According to an embodiment of the present invention, the sampling device comprises an interlock key system for preventing the simultaneous operation of the first capacitive valve and the second valve.

[0026] Preferably, the airlock is connected to a third valve for discharging the fluid, and the fluid is contained in a predetermined volume.

[0027] Advantageously, the second valve is a second capacitive valve, and the first capacitive valve and the second capacitive valve are preferably identical.

[0028] The present invention also relates to a system comprising a sealed enclosure containing solid particles and a solid particle sampling device as described above, the system being intended for one of the following applications: catalyst sampling in a petroleum refining unit, a gas or biomass treatment plant, a renewable fuel production unit, a reforming unit, a Fischer-Tropsch unit, or a unit for dehydrating alcohol to olefins.

[0029] The present invention further relates to a method for sampling solid particles from a sealed enclosure using a sampling device as described above, at least the following steps being performed: - Sampling a predetermined volume containing solid particles from the sealed enclosure through a sampling head; - Feeding the sampled predetermined volume into the capacity of a first capacitive valve in a sampling position; - Actuating the first capacitive valve to discharge a predetermined volume containing solid particles therefrom, and upon discharge of the predetermined volume, repositioning the first capacitive valve to the sampling position.

[0030] Preferably, in this method, the first capacitive valve is arranged upstream from a second capacitive valve, and when the sampling device comprises an airlock and a third valve as described above, at least the following steps are performed: - Sampling a predetermined volume containing solid particles from the sealed enclosure through a sampling head; - Feeding the sampled predetermined volume into the capacity of a first capacitive valve in a sampling position; - Actuating the first capacitive valve to discharge the predetermined volume into the airlock or directly into the second capacitive valve in the sampling position, and upon discharge of the predetermined volume, repositioning the first capacitive valve to the sampling position; - When a predetermined volume is released into the airlock, preferably, a step of releasing the fluid contained in the predetermined volume through a third valve that closes when the fluid is released after the opening; - A step of actuating a second capacitive valve to release the solid particles contained in the predetermined volume into the container, and when the solid particles are released, repositioning the second capacitive valve to the sampling position.

[0031] The present invention further relates to a method for modifying a device for sampling solid particles from a sealed enclosure, the sampling device comprising a tubular body carrying a sampling head, the sampling head being configured for gravity sampling of a predetermined volume of solid particles from the sealed enclosure, the sampling device comprising a tubular pipe, the tubular pipe being attached to the tubular body and forming a non-zero angle with respect to the tubular body, the tubular body comprising a deflector for deflecting solid particles within the tubular pipe, the sampling device comprising at least one valve downstream from the tubular pipe, the method comprising the step of replacing at least one valve downstream from the tubular pipe with a capacitive valve to obtain a sampling device as described above.

Best Mode for Carrying Out the Invention

[0032] (Brief Description of the Drawings) Other features and advantages of the device, system, and method according to the present invention will become apparent from the following description of embodiments given by way of non-limiting example with reference to the following accompanying drawings: - FIG. 1 is a partial cross-sectional view of a sampling device according to an embodiment of the present invention; - FIG. 2 is an end view of the sampling device according to the present invention in the direction of arrow A in FIG. 1; - FIG. 3 is a perspective view of the shutter means of the sampling device according to an embodiment of the present invention; - FIG. 4 shows a first type of capacitive valve of the sampling device according to the present invention; - Figure 5 shows a second type of capacitive valve of the sampling device according to the present invention, - Figure 6 shows a first embodiment of the valve assembly of the sampling device according to the present invention, - Figure 7 shows a second embodiment of the valve assembly of the sampling device according to the present invention, - Figure 8 shows a third embodiment of the valve assembly of the sampling device according to the present invention, - Figure 9 shows a fourth embodiment of the valve assembly of the sampling device according to the present invention, and - Figure 10 shows a fifth embodiment of the valve assembly of the sampling device according to the present invention.

[0033] (Detailed Description of the Invention) The terms "top", "bottom", "upper", "lower", "vertical", "horizontal" refer to a device or system in an operating position mounted in a sealed enclosure.

[0034] The terms "upstream" and "downstream" refer to the direction of flow of solid particles within the sampling device in the operating position when the sampling device is mounted in a sealed enclosure.

[0035] As used herein, a capacitive valve is a valve that includes a ball, the ball having a capacity (also called a cavity, a hollow volume) suitable for receiving an amount corresponding to the volume of the product (e.g., solid particles with or without fluid), the ball being suitable for moving between at least two positions, namely a first position called the "sampling position" where the product can be fed into the capacity and a second position called the "discharge position" where the product can be discharged from the capacity, for example under the influence of gravity.

[0036] When the capacitive valve operates under gravity, the sampling position is characterized by a capacitance arranged (at this position at the top of the ball) such that the product directly enters the capacitance forming the collection container, and the discharge position is characterized by a capacitance arranged (at this position at the bottom of the ball) such that the product is discharged from the capacitance by gravity.

[0037] By design, the capacitive valve, therefore, unlike a normal ball valve, especially valves of the prior art, is not in a situation where the product can flow freely from the inlet to the outlet. In fact, for these prior art valves (non-capacitive valves) where the ball does not have a capacitance, the product is blocked at the inlet upstream of the ball. When the valve is open (the ball is shifted), the inlet is connected to the outlet and the product can flow freely through the valve and out of the valve: in the open position, the valve allows the product to pass through. On the other hand, the capacitive valve has a sampling position where the product flows into the capacitance of the ball (in this case, the ball is connected to the product inlet) and a discharge position where the product contained in the capacitance of the ball can flow out (in this case, the ball is connected to the product outlet). For this valve type, therefore, there is no so-called "pass-through" position where the inlet and outlet of the valve are directly connected. For the same reason, the capacitive valve does not have a so-called "open" or "closed" position. The absence of such a pass-through (or open) position can limit the risk of leakage of fluids, especially gases.

[0038] In the following description, a valve referred to as "non-capacitive" is not a capacitive valve in the sense of the above definition: it thus does not have a ball with the capacity to collect solid particles, but it has a closed position in which solid particles are blocked upstream and an open-through position in which solid particles can flow from upstream to downstream of the valve through the ball.

[0039] The present invention relates to a device for sampling solid particles from a sealed enclosure. The solid particles can be, for example, a catalyst in a reactor or wheat grains in a silo. The solid particles are provided in the form of granules, extrudates or balls (minerals, sand, grain particles) or in any form that allows gravity flow.

[0040] The sealed enclosure can be a silo, a hopper, a reactor, for example, a fixed-bed or continuous-bed catalytic reactor, a regenerator or an adsorber. The enclosure can be under pressure or at atmospheric pressure.

[0041] The sampling device is intended to be used when the enclosure is in operation or when it is stopped.

[0042] The sampling device comprises a tubular body carrying a sampling head, the sampling head being configured for gravity sampling of a predetermined volume of solid particles from the sealed enclosure. In order to collect a predetermined volume of solid particles by gravity, the tubular body and the head are inclined so that the solid particles naturally fall into the tubular body under the influence of their weight. The inclination of the tubular body depends on the type of solid particles, their shape, density and, in some cases, on the fluid (gas or liquid) with which they may or may not be integrated and which facilitates their entrainment within the tubular body. Preferably, the tubular body forms an angle in the range of 30° to 90° with respect to the horizontal to facilitate the gravity movement of the solid particles.

[0043] The sampling head is inserted into the inner part of the sealed enclosure. The sampling head preferably operates according to the principle of a baffle that enables it to collect a defined quantity (predetermined volume) of solid particles and prevent a larger quantity of flow.

[0044] The sampling head can preferably comprise a cylindrical housing, which has, for example, a circular shape, with its longitudinal axis coinciding with the axis of the body, and its upper part closed by a lid and its lower part closed by a bottom. At least one recess is provided in the lid and the bottom respectively in the form of an angular sector.

[0045] The sampling head can preferably comprise a solid particle collection recess (within the sealed enclosure), a collected solid particle transfer recess, and angular displacement shutter means for these recesses, and the shutter means are controlled by control means. The shutter means can in particular comprise a cup, which is provided with an axial hollow passing through the cup, and collection of solid particles is possible when the axial hollow faces the collection recess, or transfer of solid particles is possible when the axial hollow faces the transfer recess. The transfer and collection recesses are angularly offset such that the axial hollow faces one or the other of the collection and transfer recesses and such that solid particles cannot be transferred simultaneously while other particles are being collected. Therefore, the angular offset must at least correspond to the maximum width of the recess. With a sufficient angular offset, a defined volume of solid particles can be collected, which on the one hand facilitates the release of the solid particles and on the other hand facilitates the analysis performed on the solid particles thus collected.

[0046] The control means can comprise a rod and is connected to a limiting means, for example a stopper, for limiting the angular displacement of the shutter means and / or the control means.

[0047] The rod can be connected to an operating lever that cooperates with the stopper.

[0048] The rod can be provided with a torsion spring means for the circumferential bearing of the lever with respect to one of the stoppers.

[0049] The control means can comprise a rod, be connected to the shutter means, and be provided with an end position detection device for limiting the no-load angular displacement of the shutter means, or any other mechanical actuator (pneumatic, hydraulic, electric) can be attached and connected to a geared motor having two rotational directions.

[0050] Alternatively, the control means can comprise a rod connected to the shutter means and a cam controlled by a cylinder.

[0051] According to another alternative, the control means can comprise a rod which is connected to the shutter means and carries a pinion that cooperates with a rack mounted by a cylinder.

[0052] The tubular body can be provided with an upper tubular extension suitable for being partially fitted into the enclosure, which supports the sampling head and collects solid particles from the enclosure.

[0053] The tubular body can also be provided with a lower tubular extension, which includes various means for controlling the rotation of an element (especially a cup) that enables the collection of a solid particle sample.

[0054] Preferably, the tubular body of the sampling device can be made to be reversibly attached to the tube of the enclosure and can be easily removed, replaced, or inspected.

[0055] The tubular body of the sampling device can be provided with a fixed flange, for example, intended to be assembled on the flange of the enclosure in which it is located.

[0056] Furthermore, the sampling device comprises a tubular pipe attached to the tubular body, the tubular pipe forming a non-zero angle with respect to the tubular body, and the tubular body comprises a deflector for deflecting solid particles within the tubular pipe. The tubular pipe is preferably located downstream of the tubular body in the direction of flow of the solid particles within the sampling device. Therefore, the solid particles flow from the tubular body into the tubular pipe after being deflected by the deflector under the influence of gravity. Advantageously, the tubular pipe has an angle ranging from 10° to 90° with respect to the tubular body axis, preferably from 20° to 70°, more preferably from 30° to 60°, and even more preferably from 40° to 50°.

[0057] Preferably, the lower tubular extension can comprise a deflector housed and fastened to this lower tubular extension in order to direct the sampled solid particles supplied from the tubular body towards the tubular pipe.

[0058] The deflector can preferably carry a deflection surface on which the solid particles are deflected, and the deflection surface forms an angle ranging from 0° to 60° with respect to the vertical, preferably from 5° to 45°, and more preferably from 10° to 30°.

[0059] Furthermore, the sampling device comprises a first capacitive valve (at least the first capacitive valve, preferably several capacitive valves, especially two capacitive valves) for discharging the solid particles, and the first capacitive valve (or the plurality of capacitive valves) is located downstream of the tubular pipe in the direction of flow of the solid particles within the sampling device. "Located downstream of the tubular pipe" or "downstream of the tubular pipe" means that the valve under consideration is directly (in this case, the valve is attached to this downstream end of the tubular pipe) or indirectly connected to the downstream end of the tubular pipe (the end of the tubular pipe not attached to the tubular body) by a facility providing a junction between the downstream end of the tubular pipe and the valve.

[0060] In fact, when the first capacitive valve is in the sampling position, the solid particles collected by the sampling head fall under gravity into the cavity (also called the capacitance) of the ball of the first capacitive valve. They do not accumulate on the surface of the ball upstream from the ball and providing the valve sealing on its seat. When the capacitive valve is shifted to the discharge position, the solid particles are discharged. Assuming that the solid particles are in the cavity of the ball and not on the sealing surface of the ball, the ball and the seat (providing the valve sealing) of the valve are less likely to wear during the operation of the ball. Therefore, by using a capacitive valve, wear of the ball and the seat can be limited, and in particular the risk of leakage when the enclosure is under the pressure of a liquid or a gas can be limited, and thus it becomes possible to limit the maintenance (replacement of the ball and / or the entire valve) of this material.

[0061] In addition, the design of the capacitive valve without a bypass position makes it possible to prevent leakage into the atmosphere as a result of improper handling of this valve by using the first capacitive valve on the sampling device. Thereby, it becomes possible to improve the safety of the sampling device.

[0062] Advantageously, the volume of the capacitance of one or more first capacitive valves can be made larger than a predetermined volume (captured by the sampling head). Therefore, the sampled solid particles can be completely contained within the capacitance, thereby preventing contact between the solid particles and the sealing surfaces of the ball and seat while handling the valve. Preferably, the volume of the capacitance of one or more first capacitive valves is at least 1.05 times, preferably at least 1.15 times, the predetermined volume. Therefore, the capacitance contains the total volume of the sampled solid particles and is large enough to prevent contact between the sampled solid particles and the sealing surfaces of the valve's ball and / or seat (or multiple seats if the valve has two seats). Early wear of the valve is thus avoided.

[0063] According to a first variant of the invention, the first capacitive valve (or valves) can comprise a single sheet and a capacitive ball, the single sheet being upstream of the capacitive ball. Therefore, the capacitive ball has a capacitance that allows the collection and release of solid particles. The single sheet upstream of the ball ensures the impermeability of the valve to the gas and / or liquid contained in the enclosure (i.e., the solid particles are located on the side where the fluid flows from the tubular body and then the tubular pipe), maintaining the pressure in the enclosure.

[0064] According to a second variant of the invention, one or more first capacitive valves (or valves) can comprise a first sheet, a second sheet, and a capacitive ball, the first sheet being upstream of the capacitive ball and the second sheet being downstream of the capacitive ball. Therefore, the capacitance of the capacitive ball can contain the solid particles sampled from the sampling head. The double sheets upstream and downstream improve the sealing of the valve and minimize wear.

[0065] Advantageously, one or more first capacitive valves can be selected from among capacitive spherical valves, capacitive conical ball valves, capacitive cylindrical ball valves or any similar capacitive valves. These valve types are reliable and they minimize the risk of wear.

[0066] A capacitive spherical valve is a valve in which the ball is spherical and the spherical ball has capacitance. This type of valve enables optimization of the amount of material relative to pressure and / or temperature constraints.

[0067] A capacitive conical ball valve is a valve in which the ball is conical and the conical ball has capacitance. This type of valve is easier to manufacture than a capacitive spherical valve. It may be necessary to add a lubrication system or a polymer coating.

[0068] A capacitive cylindrical ball valve is a valve in which the ball is cylindrical and the cylindrical ball has capacitance. It is the easiest capacitive valve to manufacture.

[0069] According to a preferred configuration of the present invention, the sampling device can (at least) comprise a second valve arranged downstream from the tubular pipe (connected directly or indirectly to the downstream end of the tubular pipe) for the release of solid particles from the sampling device, and the second valve is upstream or downstream from the first capacitive valve.

[0070] The phrase "the second valve is upstream or downstream of the first capacitive valve" means that the second valve is directly or indirectly connected to the upstream end of the first capacitive valve (in this case, the second valve is located between the downstream end of the tubular pipe and the upstream end of the first capacitive valve), or that the second valve is directly or indirectly connected to the downstream end of the first capacitive valve.

[0071] In other words, in the direction of the flow of solid particles within the sampling device, can the solid particles first pass through the first capacitive valve and then through the second valve, or can they first pass through the second valve and then through the first capacitive valve? However, it is more interesting to use the first version (flowing through the first capacitive valve first). In fact, the capacitive valve makes it possible to prevent wear and improve sealing, so it is advantageous for the upstream valve to be the first capacitive valve, which provides better sealing and makes it possible to avoid the risk of decompression of the enclosure. In addition, the first valve through which the particles flow is the valve that is exposed to the highest temperature, which may increase the wear of the valve.

[0072] The first capacitive valve and the second valve can be connected to each other directly or by an airlock. It can be interesting to use an airlock when it is desired to decompress the sample before collecting the solid particles in the container at ambient pressure, or to release the gas or liquid contained in the sample together with the solid particles. Therefore, it is possible to discharge a predetermined volume by means of the airlock.

[0073] An "airlock" is understood to be a hollow part, preferably tubular, suitable for containing all of a predetermined volume of solid particles.

[0074] The upstream valve (advantageously a first capacitive valve) can be directly attached to the tubular pipe.

[0075] According to an advantageous embodiment of the invention, the sampling device can comprise an interlock key system to prevent the simultaneous operation of the first capacitive valve and the second valve. In fact, when the second valve is a non-capacitive ball valve and it is in the open position (i.e., the position where the inlet and the outlet are directly connected), and when the enclosure is under pressure, the operation of the first capacitive valve can release the fluid trapped under pressure in the cavity volume, thereby potentially causing an accident.

[0076] According to an advantageous configuration of the invention, the airlock can be connected to a third valve for the release of the fluid, and the fluid is contained in a predetermined volume. In fact, the enclosure, for example a reactor, can contain, in addition to solid particles, a fluid, often a gas, such as hydrogen, hydrocarbon gas and / or nitrogen. Furthermore, this fluid is often maintained at a pressure above atmospheric pressure (e.g., at least 5 bar, preferably at least 15 bar) and / or at a high temperature (at least 40 °C).

[0077] Before collecting the solid particles, the fluid is preferably depressurized and / or released to prevent the risk of poisoning and / or explosion to the staff. By using the airlock between the first capacitive valve and the second valve (from upstream to downstream or from downstream to upstream), it becomes possible to add a line for the depressurization and / or release of the fluid (e.g., to a flare for burning the gas or to a rinsing system using an inert fluid). Then, the third valve can be set on this line. Opening the third (non-capacitive) valve allows the fluid to be released (and depressurized if necessary); closing the third valve allows the airlock to be isolated.

[0078] Preferably, the second valve can be a second capacitive valve. Therefore, the sampling device comprises two capacitive valves, one of which is directly connected (attached) to the tubular pipe and thus provides sealing with the enclosure, and the other is connected downstream directly or indirectly by an airlock. Both capacitive valves are used to release solid particles. By using two consecutive capacitive valves, it becomes possible to further limit the risk of leakage. Thereby, it also becomes possible to use a line for discharging the fluid contained in the sampled predetermined volume.

[0079] The second capacitive valve can preferably have the same characteristics as the first capacitive valve. In other words, it is as follows: - The volume of the capacitance of the second capacitive valve can be larger than the predetermined volume, preferably the volume of the capacitance of the second capacitive valve is at least 1.05 times, more preferably at least 1.15 times the predetermined volume. - The second capacitive valve can comprise a single sheet and a capacitive ball, and this single sheet is upstream from the capacitive ball. - Alternatively, the second capacitive valve can comprise a first sheet, a second sheet, and a capacitive ball, the first sheet being upstream from the capacitive ball and the second sheet being downstream from the capacitive ball. - The second capacitive valve is selected from among a capacitive spherical valve, a capacitive conical ball valve, or a capacitive cylindrical ball valve.

[0080] The body, ball and one or more sheets of one or more capacitive valves are made of materials suitable for the application, in particular the fluid, pressure and temperature present. Furthermore, the one or more sheets are made of a material with a higher elastic strength and / or hardness than the material of which the ball and body are made, limiting the wear of the one or more sheets.

[0081] Preferably, the ball and the one or more sheets can be subjected to a surface treatment, increasing the friction and its resistance to wear.

[0082] Preferably, the first capacitive valve and the second capacitive valve can be identical to simplify their design, logistics and maintenance and to prevent the risk of mixing the two valves during installation.

[0083] The invention also relates to a system comprising a sealed enclosure and a solid particle sampling device as described above, the sealed enclosure containing solid particles. This system can be intended for one of the following applications: catalyst sampling in a petroleum refining unit, a gas or biomass treatment plant, a renewable fuel production unit, a reforming unit, a Fischer-Tropsch unit or a unit for dehydrating alcohol to olefins.

[0084] Furthermore, the invention also relates to a method for sampling solid particles from a sealed enclosure using a sampling device as described above, at least the following steps being carried out: - a step of collecting a predetermined volume containing solid particles from the sealed enclosure through the sampling head (e.g. via a cup and a collection / transfer recess); - a step of sending the collected predetermined volume (containing the collected solid particles and optionally a fluid, in particular a gas) to the capacity of the first capacitive valve in the sampling position; - Operating the first capacitive valve to discharge a predetermined volume containing solid particles of the first capacitive valve, and repositioning the first capacitive valve to the sampling position when the predetermined volume is discharged.

[0085] Advantageously, when this device comprises a second capacitive valve and the first capacitive valve is arranged upstream from the second capacitive valve (preferably attached to a tubular pipe) (in other words, the collected solid particles first flow through the first capacitive valve and then through the second capacitive valve), and when the device optionally comprises an airlock and a third valve as described above, at least the following steps can be performed: - Sampling a predetermined volume containing solid particles (and optionally a fluid, especially a gas) from the sealed enclosure through the sampling head (for example, via a cup and a collection / transfer recess); - Sending the collected predetermined volume to the capacity of the first capacitive valve at the sampling position; - Operating the first capacitive valve to discharge the predetermined volume into the airlock (if the sampling device comprises an airlock) or directly into the second capacitive valve at the sampling position, and repositioning the first capacitive valve to the sampling position when the predetermined volume is discharged; - When the predetermined volume is discharged into the airlock, preferably discharging the fluid contained in the predetermined volume through a first valve that is open and will be closed after this fluid is discharged, to remove this fluid (especially if this is hydrogen), for example sending this to a flare, or depressurizing the airlock to ambient pressure before recovering the solid particles; - Operating the second capacitive valve to discharge the solid particles contained in the predetermined volume into a container, and repositioning the second capacitive valve to the sampling position when the solid particles are discharged.

[0086] In the method implemented by the sampling device according to the present invention, the collected solid particle sample is not stored upstream from one or more valves, whereby erosion of the valve seat and / or ball where the solid particles rub may be caused during transfer. The sample is stored directly in the cavity of the ball of one or more capacitive valves, thus preventing friction with the surface forming the seal when the valve is actuated.

[0087] One or more capacitive valves can be operated manually, pneumatically, electrically or automatically.

[0088] When the sampling device comprises a first capacitive valve attached to a tubular pipe, followed by an airlock and a non-capacitive second valve at the airlock outlet for releasing solid particles by gravity, and a non-capacitive third valve for releasing a fluid, e.g. a gas, the order of use of these valves can typically be as follows: - During collection of the sample in the sealed enclosure in the standby position: The first capacitive valve is in the sampling position for collecting the sample in the cavity of the valve ball, and the second and third valves are closed. In contrast to the prior art, the sample is not stored in the body of the device upstream from the first capacitive valve. - In a second step, when the sample has been collected and stored in the cavity of the first capacitive valve, this valve is rotated 180° to the discharge position, the cavity being oriented downwards while the non-capacitive second and third valves remain closed, so that the sample falls by gravity into the airlock upstream from the closed non-capacitive second valve. - The non-capacitive third valve is then opened and subsequently closed to bring the fluid originally present in the capacitor to atmospheric pressure or the pressure of the flare system. Other variations are possible by rinsing with an inert fluid and adding two more valves on the fluid circuit. - The sample is then upstream of the non-capacitive second valve at atmospheric pressure. - The non-capacitive second valve is then opened to collect the sample from the collection pot (container) by any means. - The second valve is closed and returns to the standby position: V1 is positioned so that a sample can be collected, the cavity of the shutter part faces upward in the filling position, and V2 and V3 are closed.

[0089] When the fluid is not under pressure, the use of the third valve can be avoided.

[0090] If the sampling device is provided with a first capacitive valve attached to a tubular pipe, followed by an airlock, a second capacitive valve for discharging solid particles downstream of the airlock, and a line for discharging the fluid connected to the airlock, and the line is provided with a non-capacitive third valve, the order of valve use can be as follows: - During the collection of the sample in the sealed enclosure in the standby position: The first capacitive valve is positioned to collect the sample in the cavity of the ball of the first capacitive valve, the second valve is in the sampling position, and the third valve is closed. - When solid particles are taken from the enclosure, they are generally at a high temperature and are stored in the tubular body of the device. - They are then transferred by gravity from the tubular body of the device into the cavity of the first capacitive valve rotated 180°, discharging the sample into the airlock. - Next, under gravity, the solid is transferred and stored in the cavity of the ball of the second capacitive valve. In contrast to the prior art, the sample is not stored in the upstream airlock from the non-capacitive second valve in the closed position. Erosion of this valve was possible during valve operation. - The first capacitive valve then remains in the discharge position, the non-capacitive third valve remains closed, and the second capacitive valve remains in the sampling position. - The third valve is opened and then closed so that the fluid originally present in the capacitance reaches atmospheric pressure (thus purging is performed). Other variations are possible by rinsing with an inert fluid and adding two more valves. The first capacitive valve then remains in the discharge position and the non-capacitive third valve remains closed. - The sample is at atmospheric pressure inside the cavity of the second capacitive valve. - The second capacitive valve is then rotated 180° to collect the sample into a collection pot (container) by any means, the first capacitive valve remains in the discharge position, and the third valve remains closed. - The first and second capacitive valves are then rotated 180° to place them in the collection position, and the third valve is maintained in the closed position.

[0091] In this configuration, an airlock is not essential because a predetermined volume can fall directly by gravity into the cavity of the second capacitive valve.

[0092] In addition, the use of the third valve can be avoided when the fluid is not under pressure.

[0093] The present invention also relates to a method of improving a device for sampling solid particles from a sealed enclosure. The sampling device comprises a tubular body carrying a sampling head, the sampling head being configured for gravity sampling of a predetermined volume of solid particles from a sealed enclosure (typically a reforming reactor), the sampling device comprising a tubular pipe which is attached to the body and forms a non-zero angle with the tubular body, the tubular body comprising a deflector for deflecting the solid particles within the tubular pipe, and the sampling device comprising at least one valve downstream from the tubular pipe. The improvement method comprises the step of replacing at least one valve, preferably two valves, downstream from the tubular pipe (directly or indirectly connected to the downstream end of the tubular pipe) with capacitive valves, to obtain a sampling device as described according to the present invention.

[0094] Preferably, the initial sampling device (before improvement) comprises a first valve attached to the pipe, the first valve being followed by an airlock and a second valve (downstream from the airlock), the airlock being connected to a fluid discharge line, the fluid discharge line being provided with a third valve. The improvement method then consists of replacing the first or second valve with a first capacitive valve, limiting wear of the ball and / or seat, avoiding too frequent replacement of the ball, seat, or valve, and limiting the risk of fluid leakage. Preferably, both the first and second valves are replaced with capacitive valves, further limiting the risk of fluid leakage and wear of the ball and / or seat.

[0095] FIG. 1 schematically shows a cross-sectional view of a sampling device according to the present invention as a non-limiting example.

[0096] The sampling device (10) according to the invention is arranged on an enclosure (12), in particular a reactor. The enclosure (12) is preferably sealed and advantageously isolated from the atmosphere. The enclosure contains solid particles (14) and optionally a fluid, in particular a gas. The sampling device comprises a sampling head (16) for taking a solid particle sample into this enclosure. This sampling head (16) is mounted by a tubular body (18) on the longitudinal axis XX which penetrates the wall (20) of the enclosure (12). The sampling head (16) operates on the principle of a deflector, making it possible to collect a predetermined volume of solid particles in the enclosure (12) and to avoid a large flow.

[0097] This sampling head (16) comprises a cylindrical housing (22). The cylindrical housing (22) is circular here, its longitudinal axis coincides with the axis of the tubular body (18), and it is closed at its upper part by a lid (24) and at its lower part by a bottom (26). The lid (24) and the bottom (26) are each provided with recesses (28), (28') in the form of angular sectors (the shape of which can be better seen in Figure 2). The recess (28) in the lid (24) is a collection recess for collecting solid particles from the enclosure, and the recess (28') in the bottom (26) is a transfer recess.

[0098] The inside of the cylindrical housing (22) houses shutter means. Here, the shutter means is in the form of a cup (30). The diameter of this cup (30) substantially corresponds to the inside diameter of the cylindrical housing (22), and its height is substantially equal to the height of this cylindrical housing (22), such that this cup (30) can rotate freely inside the cylindrical housing (22) and between the lid (24) and the bottom (26). This cup (30) is provided with a hollow portion (32), which is substantially parallel to the longitudinal axis and passes through the cup (30) (better visible in FIGS. 2 and 3). Advantageously, the cross-section of the hollow portion (32) is in the form of an angular sector, and its shape corresponds to the recesses (28) and (28’) of the angular sectors of the lid (24) and the bottom (26). Preferably, the dimensions and the angle of the sector of the recess (28) of the lid (24) are smaller than those of the hollow portion (32) of the cup (30), whereas the dimensions and the angle of the sector of the recess (28’) of the bottom (26) are larger than those of the hollow portion (32) of the cup (30). The volume of the cup defines a predetermined volume of the sampling head.

[0099] The tubular body (18) of the sampling device is advantageously inclined at an angle α of 45° with respect to the horizontal in the enclosure (12), facilitating the transfer of solid particles by gravity.

[0100] The tubular body (18) comprises an upper tubular extension (44), which is here circular in shape, partially penetrates inside the enclosure (12), and supports a sampling head (16) for sampling the solid particles housed in this enclosure (12). The tubular body (18) also comprises a lower tubular extension (46), which houses various means (48) for controlling the rotation of the cup (30) to enable the collection of samples.

[0101] The lower tubular extension (46) also includes a deflector (50). The deflector (50) is housed and fixed within this lower tubular extension (46), drives the collected sample towards the tubular pipe (52), and connects to valve V1 and then to the airlock (54).

[0102] The deflector (50) has a deflecting surface (56) mounted by a tubular sleeve (58) having an angle of 25° with respect to the vertical, enabling the gravitational flow of the sampled solid particles towards the airlock. This deflector (50) also includes a fastening base plate (60) on the lower end of the tubular body (18), as well as a longitudinal bore (62) starting from the deflecting surface and connecting to the base plate (60), allowing the passage of the cup rotation control means.

[0103] The airlock (54) is connected to three valves V1, V2, and V3. The tubular part (55a) connects the airlock (54) to the third valve V3 for the discharge of the fluid (a part of the sample taken together with the solid particles, and this fluid is also included in the enclosure (12)) to the flare or fluid collection line of the fluid.

[0104] Another tubular part (55) connects the airlock (54) to the first valve V1 and the second valve V2.

[0105] The tubular parts (55) and (55a) are substantially orthogonal.

[0106] The tubular pipe (52) connected to the first valve V1 is provided with a fixed flange (64) for assembly on the sole (66). The sole (66) is fastened to the outside of the wall (20) and surrounds the through hole (68) for the upper tubular extension (44).

[0107] The tubular extension (52) is oriented at a non-zero angle β with respect to the axis XX of the body.

[0108] The rotation control means (48) for the cup (30) comprises a drive rod (70) which extends from the cup (30) to the outside of the lower end of the tubular body (18) and penetrates the tubular body (18) and the deflector (50), and which is connected to an operating lever (72) arranged outside the tubular body.

[0109] The upper end of this rod (70) is connected to the cup (30) through the bore (38) by any known means, for example screwing or male-female joining, while the lower end of this rod (70) is fixedly connected to the operating lever (72), preferably by keying or screwing. Thus, by rotating the operating lever (72), a rotational movement of the cup (30) is caused.

[0110] Advantageously, by being fastened to the base plate of the deflector (50), a circular plate (74) is received between the operating lever (72) and the lower end of the tubular body (18). The fastening can be provided, for example, by a system combining a pin and a nut, which thus makes it possible to prevent the circular plate (74) from rotating when the operating lever (72) is actuated.

[0111] Furthermore, a sealing device (76) (more generally called a stuffing box) is received between the rod (70) and the bore (62). This sealing device (76) thus makes it possible to absorb the difference in temperature and pressure between the enclosure (12) and the external environment.

[0112] Furthermore, a person skilled in the art is aware of other installations which may be provided on the system, for example stuffing boxes, in particular through the information contained in patent application FR-3,007,137 A1.

[0113] To form the sampling device, the cup (30) is housed within the cylindrical housing (22). The bottom (26) is then added to this subassembly by aligning the bore (38) with the perforation (42) at the bottom (26). The lid (24) is then added by means of pins (34) that fit into the blind bore (36). The lid (24) and the bottom (26) are attached onto the cylindrical housing (22) by any known means, such as screwing or welding.

[0114] Next, an assembly consisting of a rod (70), a circular plate (74) having a stopper (not shown), a torsion spring (not shown), and an operating lever (72) for controlling the cup (30) through the rod (70) is fed into the lower tubular extension (46).

[0115] During this introduction, the end of the rod (70) is made to cooperate rotatably with the bore (38) of the cup (30) while being integral with this cup. When this is completed, the circular plate (74) is fastened to the deflector (50).

[0116] Once this assembly is formed, the tubular body (18) carrying the sampling head (16) is fed into the enclosure (12) through the through hole (68), and it is fastened onto the sole (66) by any known means, such as a screw - bolt connection. The valve V1 is then added and fastened to the tubular pipe (52) connected to the tubular body (18), and then the airlock (54) is fastened to the other end of the valve V1.

[0117] The second valve V2 is fastened downstream from the airlock (54), and the third valve V3 is fastened to the tubular part (55a) of the airlock (54).

[0118] At least one of valve V1 or V2 is a capacitive valve, preferably at least valve V1 is a capacitive valve. The capacitance of this capacitive valve (or these capacitive valves) is located within the valve ball suitable for receiving a predetermined volume of solid particles collected through the sampling head (16). Therefore, the solid particles are directly stored in the capacitance of the valve without coming into contact with the surface of the ball providing the seal and the surface of the sheet.

[0119] Preferably, both valves V1 and V2 are capacitive valves suitable for directly receiving solid particles by gravity into the cavity of the ball.

[0120] Valve V3 is intended to discharge the fluid collected with the solid particles within the enclosure. The reason this valve V3 is not a capacitive valve is that erosion does not occur due to the fluid when operating valve V3.

[0121] A pneumatic single-acting cylinder (90) can be used. This pneumatic single-acting cylinder (90) is provided with an arcuate cam (92) which is integral with the piston (94), and its stroke is limited by the structure. The return of the cylinder is provided by an integrated spring (96).

[0122] The cam (92) is in contact with the operating lever (72). When an extension from the cylinder (90) is required, the translational movement of the extension of the piston (94) occurs due to the pressure in the appropriate chamber of this cylinder, and this translational movement causes the rotation of the operating lever (72) by the cam (92) integral with the piston (94).

[0123] Since the cylinder is provided with stroke limiting means by design, the system limits the angular displacement of the operating lever (72).

[0124] Note that the sampling device can be manually operated at any timing and any operating stage of the cylinder (90).

[0125] Figures 2 and 3 schematically show, as non-limiting examples, the cup (30) and the cylindrical housing (22) of the sampling head, and the sampling head operates on the principle of a baffle that enables taking a predetermined amount of solid particles and avoiding a larger flow.

[0126] This head includes a cylindrical housing (22), which is circular here, and whose longitudinal axis coincides with the axis of the tubular body and is closed at its upper part by a lid and at its lower part by a bottom. The lid and the bottom are each provided with recesses (28), (28’) in the form of angular sectors (a) and (a’).

[0127] The inside of the cylindrical housing (22) includes a cup (30) that forms shutter means, and its longitudinal axis coincides with the axis of the cylindrical housing (22). The diameter of this cup (30) substantially corresponds to the inner diameter of the cylindrical housing (22), and its height is substantially equal to the height of this cylindrical housing (22), and this cup can rotate freely inside the cylindrical housing (22) and between the lid and the bottom.

[0128] This cup (30) is provided with a hollow portion (32), which is substantially parallel to the longitudinal axis and penetrates the cup (30). Advantageously, the cross-section of the hollow portion (32) is in the form of an angular sector (b), and its shape corresponds to the angular sectors of the lid and the bottom.

[0129] The recess (28) of the angular sector (a) of the lid and the recess (28’) of the angular sector (a’) of the bottom are offset relative to each other, offset diametrically here, so that there can be no communication through the hollow portion (32) of the angular sector (b) formed by the cup (30), and the hollow portion (32) extends axially.

[0130] Preferably, the recess (28) of the lid is formed on the angular sector (a), the angle of which is smaller than the angle of the angular sector (b) of the hollow part (32) of the cup (30). The recess (28') of the bottom is formed on the angular sector (a'), the angle of which is larger than the angle of the angular sector (b) of the hollow part (32) of the cup (30). The volume of this hollow part (32) thus makes it possible to determine a predetermined volume of the sampled solid particles.

[0131] This cup (30) is mounted on its upper surface by means of a positioning pin (34) coaxial with the axis of the cup (30), which cooperates with a blind bore provided on the inner surface of the lid. On its lower surface, the cup (30) is provided with a bore (38) intended for connection with control means (in particular a rod).

[0132] As shown particularly well in FIG. 2, the hollow part (32) of the cup can have several positions depending on the position of the operating lever.

[0133] More precisely, the hollow part (32) can have a collection position P1 in which this hollow part (32) coincides with the recess (28). In this collection position P1, a solid particle sample of the same volume as the internal volume of the hollow part (32) of the cup is transferred by gravity from the sealed enclosure into the hollow part (32) of the cup and is then closed off at its lower part by the plane of the bottom.

[0134] The discharge position P2 is here diametrically opposite to the collection position P1 and corresponds to the position in which the hollow part (32) coincides with the recess (28') of the bottom. The solid particle sample moves by gravity from the hollow part (32) into the tubular body of the sampling device, and the recess (28) of the lid is then closed by the upper surface of the cup.

[0135] The neutral position N is an intermediate position between the collection position P1 and the discharge position P2. The shown neutral position N forms an angle (d) with the collection position P1. In the shown neutral position N, the hollow part (32) does not face the recess (28) of the lid. Therefore, it is not possible to collect a sample in this neutral position N.

[0136] Figure 2 also shows the stationary position P3, where the operating lever is stationary with respect to a fixed stopper (not shown) at the position of the hollow part (32) of the cup that does not allow communication between the recesses (28) and (28’).

[0137] Therefore, there is an angular range (c), called the no-load displacement, during the rotation of the lever between the position N and the position P3, and thus of the cup, in which no solid sampling takes place.

[0138] Figure 4 schematically shows, as a non-limiting example, a first type of capacitive valve (110) for a sampling device according to the invention.

[0139] This capacitive valve (110) comprises an inlet pipe (100) and an outlet pipe (104). The inlet and outlet can of course be reversed, but for operation in gravity mode, the solid particles move by gravity and the inlet is preferably located above the outlet, and the inlet pipe (100) and the outlet pipe (104) are preferably on a vertical axis in their connection to the capacitive valve (100).

[0140] The capacitive valve (110) comprises a box (101) (also called the valve body) and is firmly attached to the inlet pipe (100) and the outlet pipe (104).

[0141] The box (101) contains a ball (102) (here a spherical ball, and the capacitive valve (110) shown is thus a capacitive spherical ball valve), and this ball (102) is movable (here rotatable) within the box (101). The rotation of the ball (102) enables the operation of the capacitive valve (110). This rotation is caused by an operating handle (105). The shaft (108) is thus firmly attached between the handle (105) and the ball (102) to function as a mechanical link between the handle (105) and the ball (102).

[0142] Preferably, the shaft (108) is in a pivotal connection about an axis (107) passing through the center of the spherical ball (102). When the handle (105) is actuated, the shaft (108) rotates about the axis (107) and rotationally drives the ball about the axis (107).

[0143] The ball (102) has a capacity (106), which consists of a hollow cavity (here a bore) within the ball (102).

[0144] The sealing of the capacitive valve (110) is provided from upstream (inlet) of the valve and downstream (outlet) of the valve through the contact between the ball (102) and a first sheet (103a) arranged upstream (thus above the ball) from the capacitive valve (110), and between the ball (102) and a second sheet (103b) arranged downstream (thus below the ball) from the capacitive valve (110).

[0145] In the position shown in the figure, the capacitive valve (110) is in the sampling position, i.e., the capacity of the ball (106) is on the opposite side of the inlet so as to enable the collection of solid particles taken through the sampling head of the sampling device under the influence of gravity. In other words, in the sampling position, the capacity (106) is arranged above the ball (102) so as to collect solid particles.

[0146] On the other hand, in the discharge position, the ball (102) is rotated 180° around the axis (107), and the capacity (106) is then below the ball (102) and discharges solid particles under the influence of gravity. The capacity (106) is here on the opposite side of the outlet of the capacitive valve (110).

[0147] This type of capacitive valve (110) with two sheets upstream and downstream improves the sealing. Furthermore, this configuration enables having an offset shaft (108) (only on the side of the ball (102)) instead of a through shaft.

[0148] Of course, the handle (105) can be replaced by other means of operating the capacitive valve (110), such as automatic - manual means.

[0149] When the capacitive valve (110) is used instead of the valve V1 in Figure 1, the inlet pipe (100) is attached to the tubular pipe (52), and the outlet pipe (104) is connected to the airlock by the tubular part (55).

[0150] When the capacitive valve (110) is used instead of the valve V2 in Figure 1, the inlet pipe (100) is attached to the tubular part (55) to connect the airlock, and the outlet pipe (104) remains empty.

[0151] FIG. 5 schematically shows, as a non-limiting example, a second type of capacitive valve (110) for a sampling device according to the present invention.

[0152] This capacitive valve (110) comprises an inlet pipe (100) and an outlet pipe (104). The inlet and outlet could, of course, be reversed, but for operation in the gravity mode, due to the transfer of solid particles by gravity, the inlet is preferably located above the outlet, and the inlet pipe (100) and the outlet pipe (104) are preferably on a vertical axis in connection with the capacitive valve (100).

[0153] The capacitive valve (110) comprises a box (101) (also called the valve body), which is firmly attached to the inlet pipe (100) and the outlet pipe (104).

[0154] The box (101) contains a ball (102) (here a spherical ball, and the capacitive valve (110) shown is therefore a capacitive spherical ball valve), which is movable (here rotatable) within the box (101). The rotation of the ball (102) enables the operation of the capacitive valve (110). This rotation is caused by an operating handle (105). The shaft (108) thus functions as a mechanical link between the handle (105) and the ball (102) by being firmly attached to the handle (105) and the ball (102).

[0155] Preferably, the shaft (108) is in a pivot connection about an axis (not shown) passing through the center of the spherical ball (102). When the handle (105) is actuated, the shaft (108) rotates about that axis, driving the ball to rotate about this axis.

[0156] The ball (102) comprises a capacitance (106) consisting of a hollow cavity (here a bore) within the ball (102).

[0157] The sealing of the capacitive valve (110) is provided only upstream (inlet) from the capacitive valve (110), through the contact between the ball (102) and the sheet (103a) located upstream from the capacitive valve (110) (and thus on top of the ball). Unlike the capacitive valve of FIG. 3, there is no sheet downstream from the ball (opposite the valve outlet).

[0158] In the position as shown in the figure, the capacitive valve (110) is in the sampling position, i.e., the capacity of the ball (106) is on the opposite side of the inlet, and under the influence of gravity, it enables the collection of solid particles collected through the sampling head of the sampling device. In other words, in the sampling position, the capacity (106) is arranged above the ball (102) to collect solid particles.

[0159] On the other hand, in the discharge position, the ball (102) has rotated 180° around the axis of the shaft (108), and then the capacity (106) is below the ball (102) to discharge solid particles under the influence of gravity. The capacity (106) is on the opposite side of the outlet of the capacitive valve (110).

[0160] This type of capacitive valve (110) with a single sheet upstream preferably has a shaft (108) passing through the ball to improve the sealing between the sheet and the ball. The shaft (108) here comprises two coaxial parts (108a) and (108b) located on either side of the ball (102). The ball (102) with the through-shaft (108) in the two parts (108a) and (108b) can be obtained, for example, by machining the ball / through-shaft assembly in one piece. The ball can also be perforated so that the two shaft parts are located on either side, and the other end of each shaft part is in rotational connection with the box (101) to enable the rotation guidance of the ball (102).

[0161] Of course, the handle (105) could be replaced by other means for actuating the capacitive valve (110), such as automatic manual means.

[0162] When a capacitive valve (110) is used instead of the valve V1 in FIG. 1, the inlet pipe (100) is attached to the tubular pipe (52), and the outlet pipe (104) is connected to the airlock by the tubular part (55).

[0163] When a capacitive valve (110) is used instead of the valve V2 in FIG. 1, the inlet pipe (100) is attached to the tubular part (55) to connect the airlock, and the outlet pipe (104) is left open.

[0164] FIGS. 4 and 5 show a capacitive ball valve, but other types of capacitive valves may be considered without departing from the scope of the present invention. For these other types of capacitive valves, the ball can be rotatably movable like the shown capacitive ball valve, or linearly movable, or movable by a combination of (one or more) rotations and (one or more) translations.

[0165] FIGS. 6 - 10 schematically show various embodiments of the valve assembly at the outlet of the tubular pipe of the device according to the present invention as non - limiting examples.

[0166] FIG. 6 shows a first embodiment of the valve assembly at the outlet of the tubular pipe.

[0167] This valve assembly comprises two capacitive valves V1 and V2, as well as a non - capacitive valve V3.

[0168] In this figure, the inlet (121) of the first capacitive valve V1 is connected to the outlet of the tubular pipe of the sampling device. In the figure, the first capacitive valve V1 is the same double-sheet valve as the valve in Figure 4. This first capacitive valve V1 is shown in the sampling position, and the capacitance is on the side opposite to the inlet (121).

[0169] The outlet (122) of the first capacitive valve V1 is attached to the airlock S1.

[0170] The airlock S1 has two other outlets: - The lower outlet of the airlock S1 for the release of solid particles by gravity; this outlet is connected to the inlet (123) of the second capacitive valve V2. - An outlet on a substantially horizontal axis for the release of fluids, especially gases, and more particularly for purging to reduce the pressure of the fluid; this outlet is connected to the tubular part (55a), to which a second tubular part (55b) is attached by a flange (120); the second tubular part (55b) is connected to a non-capacitive valve V3, which can be connected to a flare or a fluid collection tank.

[0171] The second capacitive valve V2 is the same double-sheet valve as the valve in Figure 4 and the same as the first capacitive valve V1. This second capacitive valve V2 is shown in the sampling position and has a capacitance on the side opposite to the inlet (123).

[0172] The outlet (124) of the second capacitive valve V2 is connected to a funnel (125) for discharging solid particles into the container R.

[0173] This configuration can also be obtained from the procedure for improving a sampling device in which the original non-capacitive valves V1 and V2 are replaced by capacitive valves.

[0174] To recover the solid particles collected via the sampling head of this device, the valve is operated as follows: - The capacitive valves V1 and V2 are placed in the sampling position (as shown in Figure 6), and the non-capacitive valve V3 is closed. - The solid particles and fluid that may be contained in a predetermined volume taken into the sampling head flow directly by gravity into the cavity of the first capacitive valve V1. - The first capacitive valve V1 is placed in the discharge position by rotating the ball 180°, the second capacitive valve V2 is maintained in the sampling position, and the non-capacitive third valve V3 remains closed: the solid particles then fall directly into the cavity of the second capacitive valve V2. - The non-capacitive third valve V3 is opened to release the fluid (especially gas) and / or to depressurize it, and the non-capacitive third valve V3 is closed again. During this operation, the second capacitive valve V2 remains in the sampling position, while the first capacitive valve can remain in the discharge position (preferably) or be repositioned to the sampling position. - The second capacitive valve V2 is placed in the discharge position by rotating the ball 180°. : The solid particles then fall into the funnel and subsequently into the container R, where the user can recover them; during this operation, the non-capacitive third valve V3 remains closed, while the first capacitive valve can remain in the discharge position (suitable case) or be repositioned to the sampling position. - The second capacitive valve V2 is then repositioned to the sampling position, and the first capacitive valve V1 is repositioned to the sampling position (if this operation has not been performed previously), while the non-capacitive third valve V3 remains closed.

[0175] Figure 7 shows a second embodiment of the valve assembly at the outlet of the tubular pipe.

[0176] This valve assembly comprises a single valve, which is the capacitive valve V1.

[0177] This configuration can be advantageously selected when the enclosure contains only solid particles, when it contains solid particles and a fluid at atmospheric pressure (no subsequent vacuum purge is required), and preferably when the enclosure does not contain a toxic fluid.

[0178] In this figure, the inlet (121) of the single capacitive valve V1, which is also the only valve of the sampling device, is connected to the outlet of the tubular pipe of the sampling device. In the figure, the single capacitive valve V1 is the same double-sheet valve as the valve in Figure 4. This single capacitive valve V1 is shown in the collection position, and the capacitance is on the opposite side of the inlet (121).

[0179] The outlet of the single capacitive valve V1 enables the direct release of solid particles into the container R.

[0180] In this configuration, the sampling device comprises a single capacitive valve and no non-capacitive valve.

[0181] To collect the solid particles sampled via the sampling head of the device, the single capacitive valve is operated as follows: - The single capacitive valve V1 is arranged in the sampling position (as shown in Figure 7), - Solid particles and fluids that may be contained in a predetermined volume taken into the sampling head flow directly by gravity into the cavity of the single capacitive valve V1, - The single capacitive valve V1 is arranged in the discharge position by rotating the ball 180°: The solid particles then fall directly into the container R, where the user can collect them. - The single capacitive valve V1 is then repositioned to the sampling position.

[0182] Figure 8 shows a third embodiment of the valve assembly at the tubular pipe outlet.

[0183] This valve assembly comprises a capacitive valve V1, as well as two non-capacitive valves V2 and V3.

[0184] In this figure, the inlet (121) of the first capacitive valve V1 is connected to the outlet of the tubular pipe of the sampling device. In the figure, the first capacitive valve V1 is the same double-sheet valve as the valve in Figure 4. This capacitive valve V1 is shown in the collection position, and the capacitance is on the opposite side of the inlet (121).

[0185] The outlet (122) of the capacitive valve V1 is attached to the airlock S1.

[0186] The airlock S1 has two other outlets: - The lower outlet of the airlock S1 for the discharge of solid particles by gravity; this outlet is connected to the inlet (123) of the non-capacitive second valve V2. - For the release of fluids, in particular gases, and more specifically for purging to reduce the pressure of the fluid, an outlet substantially on a horizontal axis; this outlet is connected to a tubular part (55a) to which a second tubular part (55b) is attached by a flange (120). The second tubular part (55b) is connected to a non-capacitive valve V3 and can be connected to a flare or a fluid collection tank.

[0187] The non-capacitive second valve V2 has a ball without an internal cavity.

[0188] The outlet (124) of the non-capacitive second valve V2 is connected to a funnel (125) for the release of solid particles into the container R.

[0189] This configuration can also be obtained from the results of a procedure for improving the sampling device, where the valves V1 and V2 were originally non-capacitive valves and only valve V1 was replaced by a capacitive valve.

[0190] To collect the solid particles sampled via the sampling head of the device, the valves are operated as follows: - The single capacitive valve V1 is placed in the sampling position (as shown in Figure 8) and the non-capacitive valves V2 and V3 are closed. - The solid particles and fluid that may be contained in a predetermined volume taken into the sampling head flow directly by gravity into the cavity of the single capacitive valve V1. - The single capacitive valve V1 is placed in the discharge position by rotating the ball 180° and the non-capacitive second valve V2 and the non-capacitive third valve V3 are maintained in the closed position: the solid particles then fall by gravity directly upstream from the ball of the non-capacitive second valve V2 into the airlock S1. - The non-capacitive third valve V3 is opened to release and / or depressurize the fluid (especially gas), and the non-capacitive third valve V3 is closed again; during this operation, the non-capacitive second valve V2 remains closed, while the first capacitive valve can either remain in the discharge position (preferred case) or be repositioned to the sampling position. - The non-capacitive second valve V2 is placed in the open position by rotating the ball 180°: solid particles then flow through the ball and fall into the funnel and subsequently into the container R, where the user can collect them; during this operation, the non-capacitive third valve V3 remains closed, while the first capacitive valve can either remain in the discharge position (preferred case) or be repositioned to the sampling position. - The non-capacitive second valve V2 is closed again, the first capacitive valve V1 is repositioned to the sampling position (if this operation has not been performed previously), and the non-capacitive third valve V3 is maintained in the closed state.

[0191] Figure 9 shows a fourth embodiment of the valve assembly at the tubular pipe outlet.

[0192] This valve assembly comprises a single capacitive valve V2, as well as two non-capacitive valves V1 and V3.

[0193] In this figure, the inlet (121) of the first non-capacitive valve V1 is connected to the outlet of the tubular pipe of the sampling device. In the figure, the first non-capacitive valve V1 is a double-sheet valve, but other types of non-capacitive valves could be used. This first non-capacitive valve V1 is shown in the closed position.

[0194] The outlet (122) of the first non-capacitive valve V1 is attached to the airlock S1.

[0195] The airlock S1 has two other outlets: - The lower outlet of the airlock S1 for the release of solid particles by gravity; this outlet is connected to the inlet (123) of the capacitive second valve V2, - An outlet on a substantially horizontal axis for the release of fluids, especially gases, and more particularly for purging to reduce the pressure of the fluid; this outlet is connected to the tubular part (55a), to which a second tubular part (55b) is attached by a flange (120); the second tubular part (55b) leads to a non-capacitive valve V3, which can be connected to a flare or a fluid collection tank.

[0196] The capacitive second valve V2 is the same double-sheet valve as the valve in Figure 4. This capacitive second valve V2 is shown in the sampling position, and the capacitance is on the side opposite the inlet (123).

[0197] The outlet (124) of the capacitive second valve V2 is connected to a funnel (125) for the release of solid particles into the container R.

[0198] This configuration can also be obtained from the results of the procedure for improving the sampling device, where valves V1 and V2 were originally non-capacitive valves and only valve V2 was replaced by a capacitive valve.

[0199] To collect the solid particles sampled through the sampling head of the device, the valves are operated as follows: - The single capacitive valve V2 is placed in the sampling position (as shown in Figure 9), and the non-capacitive valves V1 and V3 are closed. - The solid particles and fluid that may be contained in a predetermined volume captured by the sampling head flow directly upstream by gravity from the ball of the capacitive valve V2. - The non-capacitive first valve V1 is placed in the open position by rotating the ball, the capacitive valve V2 is maintained in the sampling position, and the non-capacitive third valve V3 remains closed: The solid particles then flow through the non-capacitive first valve V1 and fall directly into the cavity of the capacitive second valve V2. - The non-capacitive first valve V1 is closed, the non-capacitive third valve V3 remains closed, and the capacitive second valve is maintained in the sampling position. - The non-capacitive third valve V3 is opened to release fluid (especially gas) and / or to depressurize it, and then the non-capacitive third valve V3 is closed again. During this operation, the capacitive second valve V2 remains in the sampling position while the non-capacitive first valve V1 remains closed. - The capacitive second valve V2 is placed in the discharge position by rotating the ball 180°: The solid particles then fall into the funnel and subsequently into the container R, where the user can collect them; during this operation, the non-capacitive first and third valves V1 and V3 remain closed. - The capacitive second valve V2 is then repositioned to the sampling position, and the non-capacitive first and third valves V1 and V3 remain closed.

[0200] Figure 10 shows a fifth embodiment of the valve assembly at the tubular pipe outlet.

[0201] This valve assembly comprises two capacitive valves V1 and V2, which have neither an airlock nor a fluid discharge line.

[0202] This configuration is advantageously implemented when the enclosure contains only solid particles, when it contains solid particles and fluid at atmospheric pressure (no subsequent vacuum purge is required), and preferably when the enclosure does not contain toxic fluids.

[0203] In this figure, the inlet (121) of the first capacitive valve V1 is connected to the outlet of the tubular pipe of the sampling device. In the figure, the first capacitive valve V1 is the same double-sheet valve as the valve in Figure 4. This first capacitive valve V1 is shown in the sampling position, and the capacitance is on the opposite side of the inlet (121).

[0204] The outlet (122) of the first capacitive valve V1 is directly fastened to the inlet of the second capacitive valve V2.

[0205] The second capacitive valve V2 is a double-sheet valve, the same as the valve in Figure 4 and the same as the first capacitive valve V1. This second capacitive valve V2 is shown in the sampling position, and the capacitance is on the opposite side of the outlet (122) of the first capacitive valve V1 (corresponding to the inlet of the second capacitive valve V2).

[0206] The outlet (124) of the second capacitive valve V2 is connected to a funnel (125) for discharging into the container R of solid particles.

[0207] In this configuration, the sampling device comprises only capacitive valves and no non-capacitive valves.

[0208] To recover the solid particles sampled through the sampling head of the device, the valve is operated as follows: - The capacitive valves V1 and V2 are placed in the sampling position (as shown in Figure 10), - The solid particles and fluid that may be contained in a predetermined volume captured by the sampling head flow directly by gravity into the cavity of the first capacitive valve V1, - The first capacitive valve V1 is placed in the discharge position by rotating the ball 180°, and the second capacitive valve V2 is maintained in the sampling position: The solid particles then fall directly into the cavity of the second capacitive valve V2, - The second capacitive valve V2 is placed in the discharge position by rotating the ball 180°: The solid particles then fall into the funnel and subsequently into the reactor R, where the user can recover them. During this operation, the first capacitive valve V1 can remain in the discharge position (in a preferred case) or be repositioned to the sampling position, - The second capacitive valve V2 is then repositioned to the sampling position, and the first capacitive valve V1 is repositioned to the sampling position (if this operation has not been previously performed).

[0209] In Figures 6 - 10, the capacitive valve is shown as a capacitive spherical ball valve, but other types of capacitive valves could be used without departing from the scope of the invention in place of the capacitive spherical ball valve.

Brief Description of the Drawings

[0210]

Figure 1

Figure 2

Figure 3

Figure 4

Figure 5

Figure 6

Figure 7

Figure 8

Figure 9

Figure 10

Claims

**Claim 1** A device (10) for sampling solid particles (14) from a sealed enclosure (12), the sampling device (10) comprising a tubular body (18) carrying a sampling head (16), the sampling head (16) being configured for gravity sampling of a predetermined volume of solid particles (14) from said sealed enclosure (12), the sampling device (10) comprising a tubular pipe (52), the tubular pipe (52) being attached to the tubular body (18) and forming a non-zero angle with respect to the tubular body (18), the tubular body (18) comprising a deflector (50) for deflecting the solid particles (14) within the tubular pipe (52), the sampling device (10) being characterized by comprising a first capacitive valve for releasing the solid particles, the first capacitive valve being located downstream from the tubular pipe (52) in the direction of flow of the solid particles (14) within the sampling device (10). **Claim 2** The volume of the capacitance (106) of the first capacitive valve is larger than the predetermined volume, and the volume of the capacitance (106) of the first capacitive valve is preferably at least 1.05 times, more preferably at least 1.15 times the predetermined volume, a device (10) for sampling solid particles (14) from a sealed enclosure (12) according to claim 1. **Claim 3** The first capacitive valve comprises a single sheet (103a) and a capacitive ball (102), the single sheet (103a) being upstream from the capacitive ball (102), a device (10) for sampling solid particles (14) from a sealed enclosure (12) according to claim 1 or 2. **Claim 4** The first capacitive valve comprises a first sheet (103a), a second sheet (103b) and a capacitive ball (102), the first sheet (103a) being upstream from the capacitive ball (102) and the second sheet (103b) being downstream from the capacitive ball (102), a device (10) for sampling solid particles (14) from a sealed enclosure (12) according to claim 1 or 2. **Claim 5** The first capacitive valve is a device (10) for sampling solid particles (14) from a sealed enclosure (12) according to any one of claims 1 to 4, selected from a capacitive spherical valve, a capacitive conical ball valve or a capacitive cylindrical ball valve.

6. The sampling device (10) comprises a second valve downstream from a tubular pipe (52) for the release of solid particles (14), the second valve being upstream or downstream from the first capacitive valve, and the first capacitive valve and said second valve being connected to each other directly or by an airlock (S1), a device (10) for sampling solid particles (14) from a sealed enclosure (12) according to any one of claims 1 to 5.

7. The sampling device (10) comprises an interlock key system for preventing simultaneous operation of the first capacitive valve and the second valve, a device (10) for sampling solid particles (14) from a sealed enclosure (12) according to claim 6.

8. The airlock (S1) is connected to a third valve (V3) for releasing fluid, the fluid being contained in said predetermined volume, a device (10) for sampling solid particles (14) from a sealed enclosure (12) according to claim 6 or 7.

9. The second valve is a second capacitive valve, and the first capacitive valve and the second capacitive valve are preferably identical, a device (10) for sampling solid particles (14) from a sealed enclosure (12) according to any one of claims 6 to 8.

10. A system comprising a sealed enclosure (12) containing solid particles (14) and a device (10) for sampling solid particles (14) according to any one of claims 1 to 9, the system being intended for one of the following uses: catalyst sampling in a petroleum refining unit, a gas or biomass treatment plant, a renewable fuel production unit, a reforming unit, a Fischer-Tropsch unit or a unit for dehydrating alcohol to olefins.

11. A method for sampling solid particles (14) from a sealed enclosure (12) using the sampling device (10) according to any one of claims 1 to 9, the method comprising at least the following steps: - Sampling a predetermined volume containing solid particles (14) from the sealed enclosure (12) through a sampling head (16); - Sending the sampled predetermined volume to the capacitance (102) of a first capacitive valve at a sampling position; - Actuating the first capacitive valve to discharge a predetermined volume containing solid particles (14) of the first capacitive valve, and when the predetermined volume is discharged, repositioning the first capacitive valve to the sampling position.

12. A method for sampling solid particles (14) from a sealed enclosure (12) using the sampling device (10) according to claim 8, wherein the first capacitive valve is arranged upstream from a second capacitive valve, the method comprising at least the following steps: - Sampling a predetermined volume containing solid particles (14) from the sealed enclosure (12) through a sampling head (16); - Sending the sampled predetermined volume to the capacitance (102) of a first capacitive valve at a sampling position; - Actuating the first capacitive valve to discharge the predetermined volume into an airlock (S1) or directly to a second capacitive valve at the sampling position, and when the predetermined volume is discharged, repositioning the first capacitive valve to the sampling position; - When the predetermined volume is discharged into the airlock (S1), preferably discharging the fluid contained in the predetermined volume through a third valve (V3), the third valve (V3) being heated and subsequently closed when the fluid is discharged; - Actuating the second capacitive valve to discharge the solid particles (14) contained in the predetermined volume into a container (R), and when the solid particles (14) are discharged, repositioning the second capacitive valve to the sampling position.

13. A method of improving a device (10) for sampling solid particles (14) from a sealed enclosure (12), the sampling device (10) comprising a tubular body (18) carrying a sampling head (16), the sampling head (16) being configured for gravity sampling of a predetermined volume of solid particles (14) from the sealed enclosure (12), the sampling device (10) comprising a tubular pipe (52), the tubular pipe (52) being attached to the tubular body (18) to form a non-zero angle with respect to the tubular body (18), the tubular body (18) comprising a deflector (50) for deflecting the solid particles (14) within the tubular pipe (52), the sampling device (10) comprising at least one valve downstream from the tubular pipe (52), the method comprising the step of replacing the at least one valve downstream from the tubular pipe (52) with a capacitive valve (110), obtaining the sampling device (10) according to any one of claims 1 to 9.

Images