WO2023112111A1

WO2023112111A1 - Catalyst packing method and catalyst packing apparatus

Info

Publication number: WO2023112111A1
Application number: PCT/JP2021/045934
Authority: WO
Inventors: 勝彦川上; 桂清許
Original assignee: ソフタード工業株式会社
Priority date: 2021-12-14
Filing date: 2021-12-14
Publication date: 2023-06-22

Abstract

A catalyst packing method in which a catalyst (2) is scattered in a reaction tower (1) by using a rotary catalyst packing apparatus (3), wherein the catalyst (2) is supplied to a scattering device (50) disposed in the reaction tower (1), an air pressure is applied to the supplied catalyst (2) and the catalyst (2) is stirred by rotation of a stirring blade (53) of the scattering device (50) to scatter and pack the catalyst (2) in the reaction tower (1), and the packing density of the catalyst (2) in the central portion (C) in the reaction tower (1) is set to a low density and the packing density of the catalyst (2) in the peripheral portion (T) in the reaction tower (1) is set to a high density at least in the relationship between the packing density increase rate of the catalyst (2) in the peripheral portion (T) with respect to the central portion (C), the packing area of the catalyst (2) in the central portion (C) and the peripheral portion (T), and the resistance to the raw material fluid flowing through the central portion (C) and the peripheral portion (T).

Description

Catalyst filling method and catalyst filling apparatus

The present invention relates to a catalyst filling method and a catalyst filling apparatus for filling reaction towers such as petroleum refining equipment and chemical industry equipment with catalyst.

Various catalysts are used to promote chemical reactions in petroleum refining facilities and chemical industry facilities. The catalyst is shaped, for example, in the form of granules, and packed inside a reaction tower through which the raw material fluid is circulated. A catalyst filling method described in Patent Document 1 is known as a method for filling the inside of a reaction tower with a catalyst.

In the catalyst filling method described in Patent Document 1, the catalyst is densely (highly packed) in the peripheral portion inside the reaction column, while the catalyst is coarsely (low) in the central portion inside the peripheral portion. Density), and the top of the packed catalyst is formed as an angle-of-repose recess that is recessed toward the center.

In this catalyst filling method, the flow resistance of the peripheral portion is relatively increased due to the difference in catalyst packing density between the peripheral portion and the central portion, and the path of the raw material passing through the central portion is shortened. By reducing the flow path resistance, the magnitude of the flow path resistance in the peripheral portion and the central portion are made closer to each other, and the flow path resistance is made uniform.

JP-A-5-228356

By the way, in the catalyst packing method of Patent Document 1, the packing density of the catalyst in the central portion inside the reaction column is set to be high, while the packing density of the catalyst in the peripheral portion is set to be low. Since the flow resistance in the central part and the peripheral part depends on the packing density ratio and packing area ratio of the central part and the peripheral part, the resistance of the flow path in the entire inside of the reaction column is made uniform. is difficult.

For example, when operating in a low liquid hourly space velocity (about 0.2 / h) environment in a heavy oil direct desulfurization unit (RDS), if the resistance of the flow path is not uniform on the entire surface inside the reaction tower, the so-called wall effect (a phenomenon in which the raw material fluid flows more intensively at the periphery than at the center of the reaction tower), the resistance changes as the operation time increases, and the resistance at the center becomes the resistance at the periphery. , and the flow rate in the catalyst layer may be redistributed. When redistributed in this way, the flow rate of the raw material fluid flowing to the center decreases, and the heat of reaction accumulates in the center. As a result, caking of the catalyst can occur (so-called hot spots can occur). Since it is difficult to extract the solidified catalyst, the work period is extended and the cost is enormous.

An object of the present invention is to provide a catalyst filling method and a catalyst filling apparatus capable of uniforming the resistance to the raw material fluid flowing through the reactor.

The catalyst filling method of the present invention is a catalyst filling method of sprinkling a catalyst in a reaction tower using a rotary catalyst filling device, wherein the catalyst is supplied to a sprinkling device arranged in the reaction tower, and supplied Air pressure is applied to the catalyst, and the catalyst is stirred by rotation of the stirring blade of the spraying device to spread the catalyst and fill it in the reaction tower, at least in the central part of the peripheral part in the reaction tower. , the packing area of the catalyst in the central portion and the peripheral portion, and the resistance to the raw material fluid flowing through the central portion and the peripheral portion, The packing density of the catalyst in the central portion is low, and the packing density of the catalyst in the peripheral portion of the reactor is high.
According to the catalyst packing method of the present invention, since the packing density of the catalyst in the reaction column is set as described above, the resistance in the central portion and the peripheral portion in the reaction column is set equal at the desired packing density increase rate. Thus, the filling area in each of the central portion and the peripheral portion is determined so that the packing density in the central portion is low, the packing density in the peripheral portion is high, and the resistance forces in the central portion and the peripheral portion are equal. It is possible to easily uniform the resistance against the raw material fluid flowing in the reaction tower.

In the catalyst filling method of the present invention, the resistance at the central portion and the resistance at the peripheral portion are set equal to each other, and the inner diameter of the reaction column and the packing density of the catalyst with respect to the central portion of the peripheral portion are increased. The diameter of the central portion may be set in relation to the ratio.
According to such a configuration, it is possible to easily set the diameter relationship between the low-density central portion and the high-density peripheral portion.

In the catalyst filling method of the present invention, the packing density increase rate may be 10%, and the packing area ratio of the catalyst to the central portion of the peripheral portion may be 1.4 to 1.5.
According to such a configuration, the resistance force in the central portion and the resistance force in the peripheral portion can be made equal to each other, and can be made close to each other.

In the catalyst filling method of the present invention, the filling area ratio of the catalyst to the central portion of the peripheral portion may be 1.45.
According to such a configuration, the resistance force in the central portion and the resistance force in the peripheral portion can be made equal to each other.

In the catalyst filling method of the present invention, the catalyst is forcibly deposited on the peripheral portion by the sprinkling device, and the top portion of the filled catalyst has an angle-of-repose recess recessed toward the central portion. may be formed.
According to such a configuration, the central portion is filled with the catalyst that naturally falls along the angle of repose from the catalyst in the peripheral portion. can be made less dense.

The catalyst filling method of the present invention has a plurality of steps of checking the filling state of the catalyst,
The recess may be formed on the top of the catalyst in each of the plurality of steps.
According to such a configuration, since the recessed portion is formed in the top portion of the catalyst for each of the plurality of steps, the packing density in the central portion can be made lower than the packing density in the peripheral portion.

In the method for filling the catalyst of the present invention, the concave portion at the top of the filled catalyst may be filled.
According to such a configuration, by arranging the catalyst also in the concave portion at the top, the space defined by the concave portion can be effectively used for the catalytic reaction.

The catalyst filling device of the present invention is a rotary catalyst filling device that uses the catalyst filling method of the present invention described above, and includes a spraying device arranged in the reaction tower, wherein the spraying device supplies air to the catalyst. An air supply device that applies pressure, a stirring blade that rotates and stirs the catalyst to which the air pressure is applied, and a cup member in which the stirring blade is arranged and an outlet for discharging the catalyst is formed. Prepare.
According to the catalyst filling apparatus of the present invention, it is possible to exhibit the same effects as those of the catalyst filling method of the present invention described above.

Schematic diagram showing a catalyst filling device. Sectional drawing which shows a separation apparatus. Explanatory drawing which shows a catalyst filling procedure. 4 is a graph showing the relationship between the resistance force ratio to the raw material fluid and the filling area ratio of the catalyst. 4 is a graph showing the relationship between the flow velocity of the raw material fluid and the packing density of the catalyst;

[Configuration of this embodiment]
BEST MODE FOR CARRYING OUT THE INVENTION An embodiment of the present invention will be described below with reference to the drawings.
In a heavy oil direct desulfurization system (RDS), a catalyst 2 is packed inside a reaction tower 1 shown in FIG. When filling the reaction tower 1 with the catalyst 2 , a catalyst filling device 3 is introduced into the reaction tower 1 through an upper opening. The catalyst filling device 3 has a vertically extending feeder 10 and a sprinkler 50 installed at its lower end, and is vertically installed by distributor trays 4 arranged inside and outside the reactor 1. .

The supply device 10 includes a hopper 11, a separation device 20, a flow pipe 30, and a valve 40 in order from top to bottom.

The hopper 11 is arranged outside the upper opening of the reaction tower 1, stores the mixture 2B in which the catalyst 2 and the catalyst powder 2A are mixed, and can supply the mixture 2B to the separation device 20 from the lower end thereof. be. The catalyst powder 2A is dust that is smaller and lighter than the catalyst 2, and is excluded as an object to be filled in the reaction tower 1.

As shown in FIGS. 1 and 2, the separation device 20 has a triple structure of a catalyst tube 21, an inner tube 22 arranged inside the catalyst tube 21, and an outer tube 23 arranged outside the catalyst tube 21. structured. The inner tube 22 is arranged concentrically inside the catalyst tube 21 and has a space 21A between it and the catalyst tube 21 . The outer tube 23 is arranged concentrically outside the catalyst tube 21, and a storage space 23A (see FIG. 2) is provided between the outer tube 23 and the catalyst tube 21. As shown in FIG. The catalyst pipe 21 has its upper end connected to the catalyst outlet of the hopper 11 and its lower end connected to the valve 40 via the flow pipe 30 . Therefore, the catalyst 2 supplied from the hopper 11 to the valve 40 passes through the inside of the catalyst tube 21 .

A dust removal air supply pipe 24 is connected to the upper end of the inner pipe 22 . The dust removing air supply pipe 24 introduces pressurized air from an external dust removing air supply source (not shown) to the upper end of the inner pipe 22 . 1, the dust-removing air supply pipe 24 includes a horizontal pipe portion partially exposed to the outside of the outer pipe 23 and a vertical pipe portion connected to the center of the horizontal pipe portion and disposed inside the catalyst pipe 21. , but not limited to this. For example, it may be configured by an L-shaped tube having a horizontal tube portion partially exposed to the outside of the outer tube 23 and a vertical tube portion disposed inside the catalyst tube 21 . Therefore, the catalyst 2 passing through the catalyst tube 21 is sent to the valve 40 in a clean state from which the catalyst powder 2A has been removed by the dust removal air.

The outer tube 23 is a tubular body that is airtight over its entire length. A dust-removed air discharge pipe 25 is connected to the lower end of the outer pipe 23 , and an exhaust mechanism 26 for dust removal is connected to the dust-removed air discharge pipe 25 . Examples of the configuration of the exhaust mechanism 26 include a blower and a cyclone. The dust-removing air takes in the catalyst powder 2A adhering to the catalyst 2 or the catalyst powder 2A generated from the catalyst 2 when passing through the gaps of the catalyst 2 in the catalyst pipe 21, and is discharged together with the catalyst powder 2A into the dust-removing air discharge pipe. 25. In this embodiment, a suction device for sucking the catalyst powder 2A stored in the storage space 23A from the dust-removed air discharge pipe 25 and the exhaust mechanism 26 is configured. Therefore, the catalyst powder 2A taken in by the dust-removing air in the catalyst pipe 21 can be recovered by the exhaust mechanism 26 and can be discarded all at once. On the other hand, the conveyed air that has passed through the exhaust mechanism 26 is released into the atmosphere after being made into a clean state that does not contain the catalyst powder 2A.

In FIG. 2, the catalyst tube 21 has a cylindrical peripheral surface portion 21B covered with an outer tube 23. As shown in FIG. The peripheral surface portion 21B has a large number of communication holes 211 and allows ventilation between the inner surface side and the outer surface side. However, the communication hole 211 has a size or shape that does not allow the catalyst 2 to pass therethrough, but allows the catalyst powder 2A that is smaller than the catalyst 2 to pass therethrough. In FIG. 2, the catalyst tube 21 is made of a mesh material and the grid spacing is the communicating hole 211. In the present embodiment, however, a plurality of holes formed by perforating the material of the catalyst tube 21 are provided. The hole may be used as the communication hole 211 .

The inner pipe 22 has a wall portion 22C having a cylindrical portion 22A covered with the catalyst pipe 21 and an end surface portion 22B (see FIG. 1) provided at the valve 40 side end of the cylindrical portion 22A. there is The tubular portion 22A may have a plurality of fluid supply holes 221 and be ventilated between the inner surface side and the outer surface side. The fluid supply holes 221 include at least a position corresponding to a position where the first fins 80 described later are provided, and a plurality of the fluid supply holes 221 are arranged at equal intervals along the circumferential direction of the inner tube 22 . When forming the fluid supply holes 221 in the inner tube 22 by punching, the fluid supply holes 221 may be formed only at positions corresponding to the positions where the first fins 80 are provided.

A vortex generating portion 8 for generating a vortex P of a mixture 2B of the catalyst powder 2A and the catalyst 2 is provided on the inner peripheral portion of the catalyst tube 21. The vortex generator 8 has a first fin 80 whose base end is fixed to the peripheral surface portion 21B of the catalyst tube 21 and a second fin 81 whose base end is fixed to the inner tube 22 . The tip of the first fin 80 faces the downstream side in the flow direction of the mixture 2B of the catalyst powder 2A and the catalyst 2. As shown in FIG. That is, the first fin 80 slopes down from the proximal end to the distal end. The tip of the second fin 81 faces the upstream side in the flow direction of the mixed matter 2B. That is, the second fin 81 is inclined upward from the proximal end to the distal end. The horizontal position of the proximal end of the second fin 81 is the same as the horizontal position of the distal end of the first fin 80 .

Between the tip of the first fin 80 and the tip of the second fin 81, a gap S is formed for the mixture 2B to flow. The first fin 80 is formed in an annular shape around the axis of the catalyst tube 21 . The dimension between the tip of the first fin 80 and the peripheral surface portion 21B of the catalyst tube 21 is the same along the circumferential direction of the catalyst tube 21 . The second fin 81 is formed in an annular shape around the axis of the inner tube 22 . The dimension between the tip of the second fin 81 and the outer circumference of the inner tube 22 is the same along the circumferential direction of the inner tube 22 . The first fins 80 are formed in multiple stages (three stages in FIG. 2) along the axial direction of the catalyst tube 21, and the second fins 81 are formed in multiple stages along the axial direction of the inner tube 22 (in FIG. 2). 3rd stage) is formed.

In the vortex generating section 8 configured as described above, the mixture 2B, which is a mixture of the catalyst 2 and the catalyst powder 2A sent from the upstream side, especially the catalyst powder 2A, passes through the first fin 80 and the second fin 81. A vortex P is generated immediately after this.

The valve 40 is a mechanism that switches between a state of allowing the catalyst 2 to pass from the separation device 20 to the spraying device 50 and a state of blocking this. The valve 40 is opened and closed in response to a signal from the control device 5 (see FIG. 1). In addition, the control device 5 may be arranged either inside or outside the reaction tower 1 .

The spraying device 50 is connected to the lower part of the supply device 10, and is a device that rotates and sprays the catalyst 2 supplied from the supply device 10 into the reaction tower 1 as a material to be sprayed. The sprinkling device 50 has a casing 51 , a cup member 52 , a stirring blade 53 , a stirring blade driving section 54 and an air supply device 55 .

The casing 51 is a cylindrical member whose upper end is connected to the valve 40 and whose lower end fixes the cup member 52 . The peripheral surface of the casing 51 is fixed to a manway of a distributor tray 4 provided inside the reaction tower 1 . The cup member 52 accommodates the catalyst 2 sent from the valve 40 through the casing 51 .

The outer and inner circumferences of the cup member 52 are formed in a hemispherical shape, and the center of the bottom portion coincides with the axial center of the casing 51 . Further, the cup member 52 is formed with a plurality of discharge ports 52</b>B for discharging the catalyst 2 in a slit shape along the radial direction of the cup member 52 . The width dimension of the discharge port 52B may gradually decrease upward from the center of the bottom of the cup member 52, or may conversely increase gradually.

The stirring blades 53 are made of synthetic resin and arranged inside the cup member 52 . The stirring blade 53 is configured to have a plurality of stirring plate portions (blades) radially extending from a shaft portion connected to the stirring blade driving portion 54, and rotates around the shaft portion. The catalyst 2 housed in the cup member 52 is stirred. Here, the stirring blade 53 may be configured to be integrally formed with the cup member 52 and rotate together with the cup member 52, or may be formed separately from the cup member 52 and It may be configured to rotate.

The stirring blade drive unit 54 is composed of an electric motor arranged inside the casing 51 and is supported so that its axis coincides with the axis of the casing 51 . The electric motor operates based on a control signal from the controller 5 to rotate the stirring blades 53 .
A tachometer (not shown) is attached to the electric motor, and the tachometer detects the rotation speed of the electric motor and outputs a signal to the control device 5 . The control device 5 receives an output signal from the tachometer and controls the electric motor so that the stirring blade 53 reaches a predetermined number of revolutions.

The air supply device 55 is composed of an air supply source (not shown) and an air supply pipe 551 connecting the air supply source to the casing 51 . The air supply device 55 supplies air from an air supply source through an air supply pipe 551 to discharge the catalyst 2 stirred by the stirring blades 53 in the cup member 52 from the discharge port 52B.
Here, the catalyst 2 is discharged from the discharge port 52B from below to the side of the cup member 52 . The distance L over which the catalyst 2 flies in the radial direction of the reaction tower 1 can be set according to the rotation speed of the stirring blade 53, and this rotation speed is adjusted by the controller 5 that controls the electric motor. By appropriately setting the distance L over which the catalyst 2 flies in this way, it is possible to change the packing density from the central portion C to the peripheral portion T in the reaction column 1 .

[Catalyst filling method]
A method of filling the inside of the reaction tower 1 with the catalyst 2 will be described below.
[Preparation process]
First, the distributor tray 4 is assembled in the reactor 1, and the catalyst filling device 3 is installed.
[Separation process]
Next, the mixed material 2B is stored in the hopper 11, and the mixed material 2B is sent from the hopper 11 to the separation device 20. As shown in FIG. In the separation device 20, the mixture 2B sent from the hopper 11 flows downward through the space 21A between the catalyst tube 21 and the inner tube 22. As shown in FIG. Then, the mixed matter 2B flowing through the portion near the inner tube 22 of the mixed matter 2B hits the second fins 81 and its flow is obstructed, and the mixed matter 2B flowing through the portion near the outer tube 23 is blocked by the first fins 80. , it flows along the upper surface (surface) of the first fin 80 from the base end side to the tip end. A vortex P is generated immediately after the inclusion 2B separates from the tip of the first fin 80 . Due to the eddy current P, the catalyst powder 2A smaller than the catalyst 2 among the inclusions 2B flows turbulently. Accompanied by the vortex flow P, the catalyst powder 2A enters the area Q formed between the lower portions of the first fins 80 and stays therein.

Here, when the dust-removed air is sent to the inside of the inner tube 22, the dust-removed air passes through the fluid supply hole 221 located above the base end of the second fin 81, and the second fin 81 blocks the flow of the dust-removed air. The material 2B is reversed and sent to the catalyst tube 21 side, and further, the catalyst powder 2A staying under the first fin 80 is pushed out toward the communication hole 211 by the swirl P, and the catalyst powder 2A is pushed out together with the dust removal air. is stored in the storage space 23A through the communication hole 211. The catalyst powder 2A stored in the storage space 23A is sucked by the dust-removed air discharge pipe 25 and the exhaust mechanism 26. As shown in FIG.
When the storage space 23A is sucked by the dust-removed air discharge pipe 25 and the exhaust mechanism 26, a negative pressure is generated in the space 21A between the catalyst pipe 21 and the inner pipe 22, and the catalyst powder 2A in the space 21A is forcibly removed. It is sent through the communication hole 211 to the storage space 23A. Since the catalyst 2 larger than the catalyst powder 2A does not pass through the communication hole 211, it is sent downstream.

[Spraying process]
The catalyst 2 sent from the separation device 20 is sent to the spray device 50 and sprayed inside the reaction tower 1 .
First, when a signal from the control device 5 is received and the valve 40 is opened, the catalyst 2 is sent inside the cup member 52 through the casing 51 of the sprinkling device 50 . The catalyst 2 is housed inside the cup member 52 .
Air is supplied to the casing 51 by the air supply device 55 to apply air pressure to the catalyst 2 accommodated inside the cup member 52 . At the same time, the driving signal from the control device 5 is received by the agitating blade driving section 54 to operate and rotate the agitating blade 53 in the R direction to agitate the catalyst 2 and discharge it from the discharge port 52B of the cup member 52 . The discharged catalyst 2 is gradually accumulated in the reactor 1 .

The number of rotations of the electric motor, which is the stirring blade drive unit 54, is measured by a tachometer, and the measured value is sent to the control device 5. The controller 5 sends a control signal to the electric motor to rotate the stirring blade 53 at a predetermined number of revolutions (rpm). If the rotational speed of the stirring blade 53 is increased, the catalyst 2 is thrown radially outward from the cup member 52 to a large extent, while if the rotational speed is reduced, the catalyst 2 is flung small radially outward from the cup member 52 . Further, when the catalyst falling distance is long, the catalyst 2 tends to land at a position farther radially outward from the cup member 52 than when it is short.

In the present embodiment, when a predetermined amount of the catalyst 2 is filled inside the reaction tower 1 by being sprayed by the spraying device 50, the control device 5 checks the filling status of the catalyst 2 through a sensor (not shown) or the like. As a result of this confirmation, if it can be determined that the catalyst 2 has been filled as prescribed, the catalyst 2 is continued to be filled. Confirmation of the filling state of the catalyst 2 is performed by dividing it into a plurality of steps, six steps S1 to S6 as shown in FIG. 3 in this embodiment. As a plan for the demonstration test, the height of the entire catalyst 2 filled was set to 7 m, and the filling state of the catalyst 2 was checked in steps S1 to S6 for each height of 1 m. The number of steps for checking the filling state can be appropriately changed by changing the filling height of the entire catalyst 2 and the frequency of checking the filling state.

By controlling the rotation of the stirring blades 53 by the control device 5, the packing density of the catalyst 2 in the central portion C is made low, and the packing density of the catalyst 2 in the peripheral portion T is made high. The control device 5 sets at least the resistance ΔP(C) at the central portion C and the resistance ΔP(T) at the peripheral portion T to be equal to each other, and the resistance ΔP(C) and the resistance ΔP(T) are equal to each other. , and the packing density increase rate DR% of the catalyst 2 with respect to the central portion C of the peripheral portion T, the packing area of the catalyst 2 in each of the central portion C and the peripheral portion T is set, and based on this setting, the stirring blade 53 to control the rotation. In this embodiment, the catalyst 2 is a 1/16″ catalyst, the packing density increase rate is 10%, and the packing area ratio of the catalyst 2 to the central portion C of the peripheral portion T is 1.45. The relationship between the resistance force ratio (T/C) of the portion T to the central portion C and the filling area ratio (T/C) of the peripheral edge portion T to the central portion C is the relationship shown in the graph of Fig. 4. For example, When the filling area ratio (T/C) is 1.0, the resistance force ratio (T/C) is 1.7, and the resistance force ΔP (T) of the peripheral portion T becomes the resistance force ΔP (T) of the central portion C ( C) is about 170% higher than C. In this embodiment, as described above, the filling area ratio (T/C) is 1.45. 1.0, and the resistance .DELTA.P(T) and the resistance .DELTA.P(C) are set to be equal to each other.

As described above, when the packing density increase rate is 10%, the packing density of the catalyst 2 in the central portion C is made low and the packing density of the catalyst 2 in the peripheral portion T is made high (so-called Radius Grading Loading (RGL)). , the resistance of the catalyst layer in the reaction column 1 is reduced compared to packing that makes the packing density uniform between the peripheral portion T and the central portion C (so-called Dense Loading), and the operating cost of the device is reduced by about 22%. It is possible. For example, when estimated with a 50,000 BPSD (Barrel Per Stream Day) scale heavy oil direct desulfurization unit (RDS), annual operating costs of about 40 million yen or more (Feed pump, Recycle gas / Make up gas compressors) can be saved. . This will reduce _CO2 emissions by about 1,500 tons annually, contributing to the realization of a decarbonized society.

In addition, when the packing (RGL) is applied in which the packing density of the catalyst 2 in the central portion C is low and the packing density of the catalyst 2 in the peripheral portion T is high, heat of reaction is accumulated in the central portion C, and the catalyst is degraded. It is possible to suppress the formation of congealed hot spots and improve the catalytic performance.
Furthermore, compared to the central portion C, the liquid hourly space velocity LHSV of the peripheral portion T becomes smaller, and as described later, by filling the catalyst 2 while forming a recess 2C having an angle of repose, the peripheral portion The size of the catalyst 2 at T is slightly smaller than the size of the catalyst 2 at the central portion C. Taking this into account, it is predicted that the catalyst reaction rate at the peripheral edge T will be higher than at the central area C, and the catalytic activity deterioration rate at the peripheral edge T will be faster than at the central area C side. However, since the volume of the catalyst 2 is larger in the peripheral portion T than in the central portion C, there are more active points, and the amount of decrease in activity due to accelerated activity deterioration of the catalyst 2 in the peripheral portion T is originally more on the peripheral portion T side. Complement each other. Then, it is considered that the peripheral portion T and the central portion C can reach the same catalyst life. From the above, it can be said that the RGL filling of the present embodiment is a filling method that can fully utilize all catalyst performances in the reaction column 1 in addition to suppressing hot spot generation as described above.

By using the same catalyst in the peripheral portion T and the central portion C, the filling area ratio depends on the packing density increase rate DR% of the peripheral portion T and the central portion C. In the above, the catalyst 2 is 1/16″ catalyst, but the catalyst 2 is not limited to this size. 45. Further, when the packing density increase rate DR% is changed, the filling area ratio also changes. When it is 12%, the filling area ratio is 1.58.

In addition, the control device 5 controls the diameter φ(C) of the central portion C in the relationship between the inner diameter φ(Rx) of the reaction column 1 and the packing density increase rate DR% of the catalyst 2 with respect to the central portion C of the peripheral portion T. The rotation of the stirring blade 53 is controlled based on this setting. The inner diameter φ(Rx) of the reaction column 1 is 4.2 m in this embodiment, but may be 3.5 m or 5.8 m. Specifically, the diameter φ(C) of the central portion C is set based on Equation 1 below.

In this embodiment, the catalyst 2 is forcibly deposited on the peripheral edge portion T inside the reaction tower 1 by the sprinkling device 50, and the top of the catalyst 2 in each of the plurality of steps S1 to S6 for checking the filling state of the catalyst 2 , an angle-of-repose recess 2C recessed toward the central portion C is formed, as shown in FIG. The concave portion 2C is formed in a substantially conical shape with an angle of repose of about 35° to 40° with respect to the horizontal plane. Since this concave portion 2C is formed, the central portion C is filled with the catalyst 2 that naturally falls along the angle of repose from the peripheral edge portion T, so that the packing density of the central portion C can be more easily increased. can be made lower than the packing density of the peripheral portion T. Further, in this embodiment, the recess 2C at the top of the filled catalyst 2 is filled by so-called sock loading of the catalyst 2 or filling with the rotation speed of the stirring blade 53 set to 50 rpm or less. As a result, the space defined by the concave portion 2C at the topmost portion is effectively utilized for the catalytic reaction.

The graph shown in FIG. 5 shows the relationship between the packing density (g/ml) of the catalyst 2 packed in the reaction tower 1 and the flow velocity (m/sec) of the raw material fluid flowing through the reaction tower 1. The horizontal axis is the packing density (g/ml) of the catalyst 2 packed in the reaction tower 1, and the vertical axis is the flow velocity (m/sec) of the raw material fluid flowing through the reaction tower 1. As shown on the horizontal axis, the packing density (g/ml) of the catalyst 2 is low in the central portion C in the radial direction in the reaction column 1 and high in the peripheral portion T. In this embodiment, the central portion It gradually increases from C toward the peripheral edge T. Also, the flow velocity (m/sec) of the raw material fluid is indicated by an arrow in FIG. In this embodiment, since the resistance ΔP (C) and the resistance ΔP (T) are equal, the reactor 1 is operated from the initial stage of operation (SOR Start of Run) to the middle stage of operation (MOR Middle of Run). Over the latter period (EOR End of Run), drifting is unlikely to occur, the raw material fluid can be flowed over the entire interior of the reaction tower 1, reaction heat does not accumulate in the central portion C, catalyst caking can be suppressed, and catalyst Maximize performance.

After the spraying step is completed, the catalyst filling device 3 is removed from the reaction tower 1, and the raw material fluid is poured into the catalyst 2 packed inside the reaction tower 1 from the lower part of the reaction tower 1 (upstream). At this time, since the packing density gradually increases (high density) from the central side of the inside of the reactor 1 toward the peripheral side, the raw material fluid is placed at the position where the catalyst 2 is packed, for example, the reaction It flows into tower 1 whether it is on the central side or the peripheral side.
In addition, the raw material fluid may flow from the upper part of the reaction tower 1 (downstream), and in this case, the raw material fluid flows into the reaction tower 1 regardless of whether it is on the central side or the peripheral side.

In the catalyst filling method according to the present embodiment, the catalyst 2 is filled as described above. The resistance ΔP(C) and the resistance ΔP(T) of T can be made equal, thereby allowing the raw material fluid to flow over the entire interior of the reaction tower 1, preventing the accumulation of reaction heat and suppressing caking of the catalyst. can.

[Modification]
In the above embodiment, the resistance ΔP(C) at the central portion C and the resistance ΔP(T) at the peripheral portion T are set to be equal to each other. Although the filling area ratio of the catalyst 2 to C is set to 1.45, it is not limited to this, and the resistance ΔP (C) and the resistance ΔP (T) may be set close to each other.

In the above embodiment, a 1/16″ catalyst is used, but catalysts 2 of other sizes may be used. The area ratio is set in relation to the filling density increase rate DR% described above, and when the filling density increase rate DR% is set to a different value, the resistance ΔP(C) and the resistance ΔP(T) are similarly set. I wish I could.

In the above-described embodiment, the concave portion 2C having an angle of repose is formed in each of the plurality of steps S1 to S6 for confirming the filling state of the catalyst 2, but the concave portion 2C is formed only in the topmost portion of the catalyst 2 in the final step S6. may have been Further, when the central portion C and the peripheral portion T can be filled with the catalyst 2 at a desired packing density, it is not necessary to form the recesses 2C having the angle of repose.

In the above embodiment, the recess 2C at the top of the filled catalyst 2 is filled with the catalyst 2, but this filling may be omitted if the desired catalytic reaction can be obtained.

In the above-described embodiment, the discharge port 52B is formed in a slit shape along the radial direction from the center of the bottom of the cup member 52, but in the present invention, the discharge port 52B is formed between the center of the bottom of the cup member 52 and the opening edge. For example, the discharge port 52B may be composed of a plurality of holes, and these holes may be arranged side by side along the radial direction from the center of the bottom portion. Even if the discharge port 52B is formed in a slit shape, it does not need to be formed in a straight line as in the above-described embodiment, and is formed in a spiral shape from the center of the bottom of the cup member 52 toward the opening edge. It may be something to do.

In the present invention, the configuration may be such that the separation device 20 is omitted.
Even if the separation device 20 is provided, it is not limited to the configuration of the above embodiment. For example, the second fin 81 may be omitted. It is not necessary to configure the 81 from a plurality of stages, and it may be configured from a single stage.

The present invention can be used for manufacturing in the fields of metals, chemistry, and foods, and for filling catalysts 2 into reaction towers 1 of petroleum refining facilities, chemical industry facilities, and the like.

[Effect of this embodiment]
(1) The catalyst filling method of the present embodiment is a catalyst filling method in which the catalyst 2 is sprayed in the reaction tower 1 using a rotary catalyst filling device 3, and the spraying device arranged in the reaction tower 1 The catalyst 2 is supplied to the reactor 50, air pressure is applied to the supplied catalyst 2, and the catalyst 2 is stirred by the rotation of the stirring blade 53 of the spraying device 50 to spray the catalyst 2 into the reaction tower 1. At least, the packing density increase rate DR% of the catalyst 2 with respect to the central portion C of the peripheral portion T in the reaction column, the packing area of the catalyst 2 in the central portion C and the peripheral portion T, and the In the relationship between the resistance forces ΔP(C) and ΔP(T) against the raw material fluid flowing through the central portion C and the peripheral portion T, the packing density of the catalyst 2 in the central portion C in the reaction column 1 is low. , and the packing density of the catalyst 2 at the peripheral portion T in the reaction tower 1 is high. Therefore, by setting the resistance forces ΔP(C) and ΔP(T) at the central portion C and the peripheral portion T in the reaction column 1 to be equal at the desired packing density increase rate DR%, the packing density of the central portion C is Each of the central portion C and the peripheral portion T has a low density such that the filling density of the peripheral portion T is high and the resistance forces ΔP (C) and ΔP (T) of the central portion C and the peripheral portion T are equal. can be determined, and the resistance forces ΔP(C) and ΔP(T) against the raw material fluid flowing in the reactor 1 can be easily made uniform.

(2) In the catalyst filling method according to the present embodiment, the resistance ΔP(C) at the central portion C and the resistance ΔP(T) at the peripheral portion T are set equal to each other, and the inner diameter of the reaction tower 1 The diameter φ(C) of the central portion is set in relation to φ(Rx) and the packing density increase rate DR% of the catalyst 2 with respect to the central portion C of the peripheral portion T. Therefore, it is possible to easily set the diameter relationship between the low-density center portion C and the high-density peripheral portion T. FIG.

(3) The filling density increase rate is set to 10%, and the filling area ratio of the catalyst 2 to the central portion C of the peripheral portion T is set to 1.4 to 1.5. Therefore, the resistance ΔP(C) at the central portion C and the resistance ΔP(T) at the peripheral portion T can be made equal to each other and can be made close to each other.

(4) A filling area ratio of the catalyst to the central portion of the peripheral portion is set to 1.45. Therefore, the resistance ΔP(C) at the central portion C and the resistance ΔP(T) at the peripheral portion T can be made equal to each other.

(5) The catalyst is forcibly deposited on the peripheral portion T by the sprinkling device 50, and an angle-of-repose recess 2C recessed toward the central portion C is formed on the top of the filled catalyst 2. be done. For this reason, the central portion C is filled with the catalyst 2 that naturally falls along the angle of repose from the catalyst 2 at the peripheral portion T. Density can be lower than density.

(6) It has a plurality of steps S1 to S6 for confirming the filling state of the catalyst 2, and the recess 2C is formed at the top of the catalyst 2 in each of the plurality of steps S1 to S6. Therefore, since the recesses 2C are formed at the top of the catalyst 2 in each of the plurality of steps S1 to S6, the packing density of the central portion C can be made lower than the packing density of the peripheral portion T more reliably.

(7) The recess 2C at the top of the filled catalyst is filled. Therefore, by arranging the catalyst 2 also in the concave portion 2C at the top, the space defined by the concave portion 2C can be effectively used for the catalytic reaction.

(8) The rotary catalyst filling device 3 according to the present embodiment uses the catalyst filling method described above, and includes a sprinkling device 50 arranged in the reaction tower 1. The sprinkling device 50 is An air supply device 55 for applying air pressure to the catalyst 2, a stirring blade 53 for rotating and stirring the catalyst 2 to which the air pressure is applied, and the stirring blade 53 are arranged inside and discharge the catalyst 2. and a cup member 52 formed with a discharge port 52B. Therefore, it is possible to exhibit the same effects as those of the catalyst filling method described above.

DESCRIPTION OF SYMBOLS 1... Reaction tower, 11... Hopper, 2... Catalyst, 20... Separator, 21... Catalyst tube, 211... Communication hole, 21A... Space, 21B... Surrounding part, 22... Inner tube, 221... Fluid supply hole, 22A... Cylindrical part 22C Wall part 23 Outer tube

23A Storage space

2A Catalyst powder 2B Contaminants 2C Recess 3 Catalyst filling device 50 Sprinkling device 51 Casing 52 cup member, 52B... discharge port, 53... stirring blade, 54... stirring blade driving part, 8... vortex generating part, 80... first fin, 81... second fin, C... central part, P... vortex, S1 to S6 . . . step, T .

Claims

A catalyst filling method for dispersing a catalyst in a reaction tower using a rotary catalyst filling device,
The catalyst is supplied to a sprinkling device arranged in the reaction tower, air pressure is applied to the supplied catalyst, and the catalyst is agitated by the rotation of the stirring blades of the sprinkling device to spray the catalyst and the reaction. filled in the tower,
At least, the packing density increase rate of the catalyst with respect to the central portion of the peripheral portion in the reaction column, the packing area of the catalyst in the central portion and the peripheral portion, and the raw material fluid flowing through the central portion and the peripheral portion A catalyst packing method in which the packing density of the catalyst in the central portion of the reaction column is low and the packing density of the catalyst in the peripheral portion of the reaction column is high in relation to resistance.
The resistance force at the central portion and the resistance force at the peripheral portion are set equal to each other,
The catalyst filling method according to claim 1, wherein the diameter of the central portion is set in relation to the inner diameter of the reaction tower and the packing density increase rate of the catalyst with respect to the central portion of the peripheral portion.
The filling density increase rate is 10%,
3. The catalyst filling method according to claim 1, wherein a filling area ratio of the catalyst to the central portion of the peripheral portion is 1.4 to 1.5.
4. The catalyst filling method according to claim 3, wherein a filling area ratio of the catalyst to the central portion of the peripheral portion is set to 1.45.
The catalyst is forcibly deposited on the periphery by the spraying device,
The catalyst filling method according to any one of claims 1 to 4, wherein the top portion of the filled catalyst is formed with an angle-of-repose recess recessed toward the center portion.
Having a plurality of steps of checking the filling status of the catalyst,
6. The catalyst filling method according to claim 5, wherein the recess is formed on the top of the catalyst in each of the plurality of steps.
7. The method of filling the catalyst according to claim 5, wherein the recessed portion at the top of the filled catalyst is filled.
A rotary catalyst filling device using the catalyst filling method according to any one of claims 1 to 7,
A sparging device arranged in the reaction tower,
The spraying device includes an air supply device that applies air pressure to the catalyst, a stirring blade that rotates and stirs the catalyst to which the air pressure is applied, and an exhaust that has the stirring blade disposed therein and discharges the catalyst. and a cup member having an outlet formed therein.