JP2939178B2 - Method for smoothing particle filling surface in particle filling device - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a filling surface for filling particles such as catalysts, grains and feeds into a reaction vessel or a storage silo by using a particle dispersing device and a particle filling device having a filling monitoring monitor. The present invention relates to a simple smoothing method, and particularly to a method for filling a catalyst in a reaction vessel represented by a petroleum refining facility by using a particle filling apparatus having a particle dispersion apparatus and a filling monitoring monitor. The present invention relates to a method for smoothing a surface.

[0002]

2. Description of the Related Art For example, a catalyst is used for synthesizing and decomposing various materials. As an example, in the petroleum industry,
In many cases, a catalyst is used, such as a method of using a heavy gas oil as a raw material to produce gasoline having a high octane number, or a method of simultaneously performing desulfurization and decomposition using a catalyst in the presence of a large amount of hydrogen. As the catalyst, in the catalytic cracking method, for example, solid acidic silica, alumina catalyst, zeolite catalyst and the like are used. Generally, diameter: 0.5 mm to 3.0 m
m, a column having a length of 3.35 mm to 10 mm or a cross-section having three to four circles stacked on each other is used, and a carrier such as alumina, alumina-silica, zeolite or silica having the above size is used. What supports an active metal is used. In such a case, the reaction vessel (packing tower) is filled with the catalyst. However, since the state of the catalyst influences the efficiency of the operation, a catalyst spraying device is installed at the upper center of the reaction vessel in order to achieve uniform filling. Spray filling is performed to allow the catalyst to spatially drop from there.

[0003] However, even if the spray filling is carried out, the particle filling surface generally undulates in an uneven shape, and a flat filling surface cannot be obtained.
If the unevenness exceeds a prescribed level, the operating efficiency is reduced. Therefore, it is necessary to correct the unevenness by controlling the spraying parameters provided in the filling device. In particular, in the case of a catalyst, it is necessary to idealize the spatial existence density of the catalyst and to control the filling speed within a range of dens loading (high-density filling of the catalyst with the catalyst axial direction as a horizontal plane) on the filling surface. Conventionally, it is not easy to measure the unevenness of the filling surface of the dispersed particles because the depth of the reaction vessel is deep, and an appropriate measurement point is selected by a tape measure from the installation surface of the filling device and measured by actual measurement. The measurement was performed, for example, once every 30 minutes and with 12 measurement points. Therefore, it takes time to measure and is rough, and the measurement accuracy is poor, ± 50 mm
And the distribution of the filling surface was 400 mm at the maximum. The filling operation had to be stopped for each measurement, and the filling operation efficiency was poor.

[0004] Therefore, there has been a demand for the development of a technique for more accurately monitoring and measuring the unevenness of the filling surface in real time, in order to make the filling surface of the particles dispersed in the container uniform, prior to that. For example, when the catalyst is filled, a measurement accuracy of ± 20 mm of the unevenness of the filling surface has been required. In response to these demands, the present inventors first measured the deposition height by triangulation by detecting reflected light from operating points at regular intervals while scanning the particle filling surface in the container with laser light. We developed a method to do it. This method scans the filling surface with laser light when filling particles into the container, detects reflected light, and triangulates from the specific scanning point position, laser light emission position and laser light detection position at the time of measurement. The deposition height is measured, and at that time, the beam diameter of the laser beam is selected to be equal to or larger than the cross-sectional area of the particles and according to the target accuracy. A laser beam generated from a scanning device and a scanning point and a laser beam having a laser beam diameter larger than the cross-sectional area of the particles and selected according to the target accuracy for scanning the particle-filled surface with the laser light, which is mounted at a standard level An imaging device that detects reflected light, and a calculation device that calculates the depth of the scanning point by trigonometry from the position of the specific scanning point at the time of measurement, the position of the laser light generation and the position of the scanning device, and the position of the imaging device. , Charge Using the fill Monitor and a display device for displaying data including the surface depth distribution.

Thus, when filling the container with particles, the particle-filled surface is scanned with laser light, reflected light is detected, and the deposition depth of each scanning point is measured by a triangular method at a predetermined number of measurement points at predetermined measurement intervals. In addition, it is possible to display the filling surface information including the height distribution of the filling surface, an arbitrary cross-sectional trend passing through the center, and the like in real time.

[0006] On the other hand, many types of particle dispersing devices have been used. For example, it has a side slit with an adjustable opening and closing door and a lower slit on the bottom surface, a rotating disk is attached to the bottom surface, and the spraying state is adjusted by adjusting the opening of the side and lower slits and the number of rotations of the rotating disk. A type that can be controlled is used.

Another example of a particle (catalyst) spraying apparatus is as follows.
There are Densi Cat system, UOP system and COP system. Each system has a hopper and a blade for spraying catalyst. The Densi Cat method uses multiple rubber blades and is an omnidirectional uniform spraying system based on the blade opening and scattering by the blades. The UOP system utilizes the centrifugal force of two to four straight blades. The COP method uses a 1 to 3 layered blade with a guide on an elliptic plate, and has a distribution of scattering distance. In addition, 1-228
No. 07 suspends the catalyst discharger in the reaction tower so as to be able to move up and down, and raises the catalyst discharger so that the distance between the catalyst discharger and the particle packing surface falls within a predetermined distance range. Disclose a method of sequentially filling, as a catalyst filling device used therein, put a catalyst discharger composed of a motor and a shallow dish-shaped member that is rotationally driven by a motor on a gondola suspended in a reaction tower, It describes a catalyst filling device in which the shaped members have raised wear provided at predetermined intervals and slits provided between these wears.

[0008] In the art, in connection with the transport of particles, the particles are not damaged or destroyed, and a flat particle-filled surface (uniform distribution of the particles), easy, simple controllability, and easy control. There is a demand for a new particle dispersion method that can achieve handling / installability and high-speed particle transport, and also enables uniform spatial existence density of particles and high-density packing of particles (densloading). . For example, the following items are required: (b) Easy handling and installation: Setting time should be as short as possible (within 1 hour). (B) Do not damage the particles when filling. (C) Uniformity of particle filling surface: Dens loading and uniformity. (D) Filling speed: high-speed particle transport (1 ton / 5 min).

In response to such a demand, the present inventor has recently
In a particle dispersing device with a very simple structure provided with a uniaxial spheroidal disk having a slit on the lower side of the hopper, a particle dispersing device capable of solving such a problem was successfully developed by devising a slit shape. The apparatus includes an outer cover, a hopper supported inside the outer cover by the outer cover and having an open lower end, a motor having a rotating shaft supported by the hopper and extending outwardly from the opening through the center of the hopper. A uniaxial spheroid disk fixed to the lower end of the motor rotation shaft and receiving particles falling from the hopper, wherein the uniaxial spheroid disk is formed with a slit for discharging particles, and the shape of the slit is uniaxial. Particles falling from the hopper into the center area of the spheroidal disk receive rotational force from the disk and move until they reach the number of rotations of the disk. Slit shape represented by the sum of the function of the trajectory whose delay angle in the direction corresponds to the required amount of particles sprayed from its radial position toward the filling surface It is characterized in that it.

[0010]

However, it is very difficult to achieve a smooth particle-filled surface even with a particle-filling device having such a particle-dispersing device and a filling monitoring monitor. In the art, using such devices,
There is a need to establish a method for easily realizing the smoothness of the particle-filled surface.

[0011]

SUMMARY OF THE INVENTION The present inventor has determined that when spraying under constant conditions, a particle sprayer having a parameter capable of forming a mortar-like filling surface and controlling the mortar-like size is provided. It has been confirmed that the particle filling apparatus including the apparatus and the filling monitoring monitor can easily realize the smoothing of the particle filling surface by gradually reducing the size of the mortar. Based on this finding, the present invention relates to a continuous application of a particle dispersing device having a parameter capable of forming a mortar-shaped filling surface and controlling the mortar-shaped size when spraying in a constant state. A method for smoothing a particle-filled surface in a particle-filling device having a filling monitoring monitor capable of grasping the entire filling surface, wherein the filling monitoring monitor continuously grasps the state of formation of the filling surface, A mortar-like filling surface is formed by spraying in a constant state with a scatterer, and the parameters of the particle scatterer are intermittently or continuously controlled to gradually reduce the mortar-like size to form a mortar-like filling. Provided is a method for smoothing a particle-filled surface in a particle-filling apparatus, characterized by sequentially depositing filled surfaces at predetermined intervals or continuously inside the surface and smoothing the filled surface. This place
In this case, particles are scattered in the filling container in a constant state for a fixed time, and the height of the center of the mortar-shaped filling surface (h (c
When the ratio of (t)) to the height (h (edge)) of the surrounding filling surface is expressed as (h (edge) / h (ct)), a constant value is obtained by controlling the parameters of the particle scattering device. The shape of the mortar-shaped filling surface formed by spraying in the state
≧ h (edge) / h (ct) ≧ 1 . Operation of smoothing of particle packing surface of this may be repeated. A useful example of a particle is a catalyst.

[0012] As the particle dispersing device, any device that can form a mortar-shaped filling surface when spraying in a constant state and has a parameter that can control the size of the mortar is used. can be, especially when the maximum dispersion distance of the particles perform spray of particles to fill the container in a state such that the wall of the charging container, it is possible to form a cone-shaped filler surface and subjected to spraying in a constant state formation The shape of the mortar-shaped filling surface is 2 ≧ h (edge)
/ H (ct) ≧ 1 can be used. The preferred example is provided with a side slit having an adjustable opening / closing door and a lower slit on the bottom surface, a rotating disk is attached to the bottom surface, and spraying is performed by adjusting the opening degree of the side and lower slits and the rotation speed of the rotating disk. A type whose condition can be controlled, and an outer cover, a hopper supported by the outer cover inside the outer cover and having an open lower end, and supported by the hopper and extending outwardly from the opening through the center of the hopper. A motor having a rotating shaft, and a uniaxial spheroid disk fixed to the lower end of the motor rotating shaft and receiving particles falling from the hopper, wherein a slit for discharging particles is formed in the uniaxial spheroid disk, In this case, the shape of the slit is such that the particles dropped from the hopper into the central region of the uniaxial spheroidal disk receive the rotational force from the disk and rotate. Particles that are scattered from the radial position toward the filling surface from the radial position to the movement trajectory of the particles moving until the rotation speed of the disk is reached, and the delay angle in the rotation direction with respect to the movement distance in the radial direction from the center of the disk It is of the type that has a slit shape expressed by the sum of a trajectory function that matches the required amount.

As the filling monitoring monitor, any monitor such as a television type monitoring device which can continuously grasp the entire filling surface can be used. Mounted on a standard,
Generation of laser light having a laser light beam diameter greater than the cross-sectional area of the particles and selected according to the target accuracy for scanning the particle-filled surface with laser light, and a scanning device and imaging for detecting laser reflected light from a scanning point Apparatus, a specific scanning point position at the time of measurement, a calculation apparatus for calculating the scanning point depth by trigonometry from the laser light generation and scanning apparatus position and the imaging apparatus position, the filling surface depth distribution And a display device for displaying data including a laser scanning type.

In operation, a particle-dispersing device having parameters capable of forming a mortar-shaped filling surface when spraying in a constant state and capable of controlling the size of the mortar-like shape, and a continuous filling surface. In a particle filling apparatus provided with a filling monitoring monitor capable of grasping the size, the size of the mortar-shaped filling surface to be deposited is gradually reduced. That is, while continuously grasping the state of formation of the filling surface with the filling monitoring monitor, the particle spraying device performs spraying in a constant state to form a mortar-shaped filling surface, and the parameters of the particle scattering device are intermittently changed. By continuously or continuously controlling the size of the mortar shape, the filling surface is sequentially deposited at predetermined intervals or continuously inside the mortar-shaped filling surface, and the filling surface is smoothed. This smoothing operation may be repeated.

[0015]

DESCRIPTION OF THE PREFERRED EMBODIMENTS Hereinafter, a case where catalyst particles are dispersed and filled in a reaction vessel will be described as an example. FIG.
(A) is a spraying device 3 installed at the center of the upper part of the reaction vessel 1 and spatially spraying and filling the catalyst particles C;
1 shows a filling device 2 including a filling monitoring monitor 4 for continuously monitoring the state of a filling surface S of formed catalyst particles. If the spraying device 3 is of a type having a parameter (for example, rotation speed) capable of forming a mortar-shaped filling surface when spraying in a constant state and controlling the size of the mortar-like shape, , Any of which can be used. In particular, when the catalyst particles are sprayed on the reaction vessel 1 in a state where the maximum scattering distance of the catalyst particles C becomes the wall surface of the reaction vessel 1 at the filling surface, a mortar-shaped filling surface can be formed and The spraying device 3 having a parameter capable of controlling the size of the sprayer can be preferably used. Further, the particle scattering device 3 controls the parameters of the particle scattering device to form a mortar-shaped filling surface formed by performing spraying in a constant state in a range of a height at which the filling container is filled with particles. To 2 ≧ h (edg
e) Use a particle dispersing device that is easy to control in the range of / h (ct) ≧ 1 . Smoothing the shape of the bowl-shaped filling surface is made forms the filling surface deviates from this range it becomes difficult, especially h
When (edge) / h (ct) <1, it is almost impossible to smooth the filling surface. Also, h (edge) / h
When (ct) = 1, h (edge)
/ H (ct) <1 is conceivable, so if possible, it is preferable to perform 2 ≧ h (edge) / h (ct)> 1. That is, the shape of the filling surface formed by spraying is smoothed while varying between 2 ≧ h (edge) / h (ct) ≧ 1. Where h
(Edge) / h (ct) is the height of the center of the filling surface (h (h ( c
t)) and the height (h (edge)) of the peripheral filling surface (h (edge) / h (ct)) (FIG. 10).
(B)). As the filling monitoring monitor 4, any type can be used as long as it can continuously grasp the entire filling surface S.

FIG. 5 shows an example of such a spraying device 3,
(A) shows the side view and (b) shows the bottom slit. Four side slits 21 are provided on the side surface of the spraying device, and a lower slit 23 shown in FIG. A rotating disk 24 is attached to the bottom surface. Adjustable door 2 on the side slit
5 are provided. Also, the lower slit 23 can be adjusted. The spraying state can be controlled by adjusting the degree of opening of the side and lower slits and the number of rotations of the rotating disk based on the obtained filling surface information.

Returning to FIG. 1, for example, a television monitor may be used as the filling monitor 4, but here a laser generator and a laser mounted on the reaction vessel wall at substantially the same level as the spraying device 3 are used. A laser scanning type including a scanning device 5 and an imaging device 9 is illustrated. The laser generation and scanning device 5 generates a scanning laser beam 6. The imaging device 9 detects the laser reflected light within a predetermined visual field. Further, a computer 11 as a calculating device for calculating the depth of the filling surface at the scanning point by trigonometry from the position of the specific scanning point at the time of measurement, the position of the laser beam and the position of the scanning device, and the position of the imaging device, and the filling surface depth A CRT 13 as a device for displaying data including the distribution is installed in a monitoring room at an appropriate position outside the reaction vessel, and is connected to a laser generation / scanning device and an imaging device by a signal line 15. FIG. 1 (b)
Is a sectional view of the filling surface S viewed from below the level of the spraying device 3, the laser generation and scanning device 5 and the imaging device 9, and shows a state of scanning the filling surface S by the scanning laser beam 6. FIG.
Monitoring of the filling surface is performed by detecting reflected light at scanning points at regular intervals while scanning the filling surface from one end to the other with the scanning laser beam 6 from side to side.

FIG. 2 shows how the laser generating and scanning device 5 and the image pickup device 7 are attached to the container wall. The laser generation and scanning device 5 includes an appropriate laser source 7 such as a He-Ne laser or a semiconductor laser, and a laser scanner 8 that scans the filling surface with laser light back and forth and right and left. The emission direction of the laser beam can be changed by sequentially changing the inclination of optical means such as a prism. The laser source 7 and the laser scanner 8 are arranged inside the dustproof cover 17 connected to the air line 16 and directly below the dustproof cover 17 as dustproof measures because dust of the catalyst is generated during the filling of the catalyst particles. It is always blown out through the cover 17. The dust cover 17 is attached to the wall of the reaction vessel by an appropriate fixture 18. The imaging device 9 is typically a CCD
The camera 10 is disposed inside a dust-proof cover 19 also connected to the air line 16, and attached to the reaction vessel wall by a fixing bracket 20. These are supported on a tray that supports a filling device (not shown) at the center.

The field of view of the camera is the inner diameter of the reaction vessel, CCD
For example, the inner diameter of the reaction container is 4 m, the size of the CCD imaging surface is イ ン チ inch, and the focal length f = 12 mm. If the collected image, the vertical view is the filling surface distance:
At -10 m, it becomes 3 m and at filling surface distance: -5 m, it becomes 1.5 m, and there may be situations where the whole view inside the reaction vessel cannot be monitored in the entire time range. In such a case, multiple cameras and possibly multiple laser generating and scanning devices may be used. For example, when a 9 mm focal length imaging lens is used, a 4 camera × 2 laser system, a 3 camera × 1 laser system, or the like can be considered. FIG. 3 shows a 4 camera × 2 laser system. The -5 m field and the -10 m field are indicated by dotted lines. The 4-camera × 2-laser system allows a wider camera-laser interval than the 3-camera × 1-laser system, and allows for a wide range and high-precision measurement.

In measuring the filling surface by scanning with a laser beam, it is necessary that the laser beam surely reaches the filling surface at the bottom of the container. That is, it is necessary to prevent the laser beam from being interrupted by the catalyst particles falling in the container space. The size of the catalyst particles is, for example, 1.27 mm
Diameter x 3 mm length, 2.12 mm diameter x 5 mm length, filling amount is, for example, 600 mm / hour, and distance from the filling container to the lowermost layer of the filling surface is, for example, 10 m. As a result of a trial calculation of the particle existence probability, it was found that the laser beam was interrupted by the catalyst particles about once every several seconds with a laser beam having a small diameter. It has been confirmed that the filling surface can be measured by scanning with a laser beam by setting the laser beam diameter to be equal to or more than the cross-sectional area of the catalyst particles, preferably 10 times or more. The upper limit of the laser beam should be determined from the required measurement accuracy (several cm or less) and the brightness of the spot of the laser scanning point. For the purpose of the present invention, the upper limit is usually 2 to 3 cm in a normal reaction vessel. For example, to achieve an accuracy of 5 cm, the upper limit of the diameter of the laser beam is 3 cm. Here, the cross-sectional area of the catalyst particles is the maximum projected area of the particles (the maximum value of the area of the shadow formed when the particles are irradiated with parallel light).

The control of the laser scanner, the image processing from the imaging device, and the triangulation calculation are performed by a dedicated computer. The processed data is stored in a storage machine such as a magnetic disk or a magneto-optical disk and is displayed on a CRT screen in real time. Various filling information can be displayed on the CRT screen. FIG. 4 is a basic screen configuration diagram of the filling surface monitor as an example. The distribution state of the filling surface, the filling surface display of the selected specific cross section, and the like are displayed in real time. Based on the filling surface distribution information obtained in this way, the state of distribution from the filling device is corrected so that the distribution of the filling surface is constant.

FIGS. 6 to 8 show the above-mentioned Densi Cat type, UOP type and COP type spraying apparatuses for reference. Both systems have a hopper and vanes for spraying the catalyst. The Densi Cat method uses multiple rubber blades and is an omnidirectional uniform spraying system based on the blade opening and scattering by the blades. The UOP system utilizes the centrifugal force of two to four straight blades. The COP method uses a 1 to 3 layered blade with a guide on an elliptic plate, and has a distribution of scattering distance.

Referring to FIG. 9, as mentioned earlier,
Another example of a spraying device newly developed by the inventor and preferred for use in the present invention is shown. The particle scattering device 3 has an outer cover 32. At the center inside the outer cover 32, a hopper 33 is supported by the supporting means 38 from the outer cover. The hopper 33 is connected to a stocker (not shown) by a hose 40.
A motor 35 having a rotating shaft 34 is mounted on the hopper. The rotation shaft 34 extends outward from the lower end opening of the hopper 33 through the center of the hopper. An opening in the lower end of the hopper around the rotation shaft 34 constitutes an orifice 39 for dropping particles. A rotating disk 36, which makes up almost half of the uniaxial spheroid, is secured to the lower end of the motor rotating shaft 4 head-down and receives particles falling from the hopper. In the illustrated example, the rotating disk is closed leaving an opening into which the orifice 39 fits. A slit 37 for discharging particles is formed on the bottom surface of the rotating disk 36. In this case, the shape of the slit matches the number of rotations of the disk when the particles dropped from the hopper at the center of the uniaxial spheroidal disk receive rotational force from the disk. The sum of the movement trajectory of the particle moving up to and the function of the trajectory whose delay angle in the rotational direction with respect to the movement distance in the radial direction from the center of the disk matches the required amount of particles scattered at that radial position It is formed so that it may become the locus represented by.

The diameter of the orifice is exchangeable, and its maximum conductance is 80% of the slit conductance of the rotating disk in order to prevent particles from staying on the rotating disk.
It must be: The hopper size is determined by the orifice diameter. As the motor, either an electric motor or an air motor can be used, and it is desired that the motor has a sufficient torque. It is preferable that the control of the number of revolutions is performed by using a servo method or the like, and is programmable so that the number of revolutions can be minutely changed (inching) during filling to smooth the filling surface. Also, inching is effective as a simple and efficient method to cover the deviation caused by the fact that the slit provided on the uniaxial spheroid disk obtained by numerical analysis has a slit width that is not a perfect ideal shape. It is.

The shape of the rotating disk and the slit is such that the vertical spatial existence distribution of the particles immediately below the rotating disk of the particles becomes a quadratic geometric series or a secondary distribution with respect to the horizontal direction. It is necessary to do so. The shape of the rotating disk must be a uniaxial spheroid in cross section, and a = b, c <
a, preferably 0.3a <c <a, more preferably 0.5a <c <a (where a and b are radii (long axis and short axis) of a uniaxial spheroidal disc and c is uniaxial rotation Height (depth) of the elliptical disk). It is necessary for the particles to climb on the disk by centrifugal force. With other shapes, uniform dispersion becomes impossible, and the particles tend to stay. Regarding the shape of the slit, the shape of the slit on a certain (r, θ, z) is such that its area is a quadratic function of r (r ² +
d, r ² + er + f) is required, and the shape takes a shape in which the particle transfer curve is superimposed. An appropriate number of slits are provided according to the size of the disk and the spraying ability so as to uniformly disperse the particles.

In order to improve the particle scattering performance,
(A) installing a dispersion plate 41 adjacent to the bottom of the disk on the rotating shaft; (b) covering and sealing the rotating shaft with an outer sheath 42 at least inside the hopper to prevent particle destruction; c) The hopper is tiltably or movably supported from the outside by an actuator 43 so that the uniaxial spheroidal disk surface can be tilted or moved, and (d) the outer cover is provided with fixing legs 44.
(E) Modifications, such as mounting a hanger 31 on the top of the outer cover, can be used. When the dispersing plate 41 is provided, an effect of uniformly dispersing the particles without exerting a shearing force or an impact force on the particles is exerted. However, the dispersion plate is attached to the rotating shaft seal portion and does not rotate. Preferably, the rotating shaft is covered and sealed with a flexible outer sheath 42 at least inside the hopper in order to prevent breakage of the particles. More preferably, the inclination of the rotating disk surface can be adjusted and controlled (+ 15 ° to −15 °), or the rotating disk surface and the orifice can be relatively moved. When the rotating disk surface is tilted, the hopper and the rotating disk can be tilted together with the actuator 43 to adjust the tilt of the particle surface. It is appropriate to use a partial spherical joint as the actuator 43, and it is preferable that the center of the inclination coincides with the center of the rotating disk (uniaxial spheroid). This is to prevent the scattering center of the particles from shifting. In the case of movement, for example, a cylinder-piston type moving means is employed as the actuator 43. Motorized,
Any air type can be used. As the suspension mechanism,
It is preferable to use an appropriate lifting device equipped with a hook, and to use the fixing leg 14 in order to prevent swinging during suspension. The fixing leg can be built-in, and for example, an open leg type, a sansui type, or the like is adopted according to the structure of the packed tower.
Further, the fixing legs are preferably replaceable.

However, even in a particle filling apparatus having such a particle dispersion apparatus capable of adjusting the dispersion parameters and a filling monitoring monitor capable of continuously monitoring the filling surface, the smoothing of the particle filling surface is realized. It is very difficult. In the art, there is a need to establish a method for easily smoothing the particle-filled surface using such a device. In accordance with the present invention, particle spraying having a parameter that can form a mortar-like filling surface when spraying under constant conditions (eg, under uncontrolled conditions) and that can control the mortar-like size. In a particle filling apparatus provided with an apparatus and a filling monitoring monitor, smoothing of the particle filling surface can be easily realized by gradually reducing the size of the mortar. While continuously grasping the state of formation of the filling surface with the filling monitoring monitor, the particle spraying device forms a mortar-shaped filling surface by spraying in a constant state, and then intermittently or intermittently sets the parameters of the particle scattering device. The size of the mortar-like shape is gradually reduced by continuous control, and the filling surfaces are sequentially deposited at predetermined intervals or continuously inside the mortar-like filling surface, thereby smoothing the filling surface. This smoothing operation may be repeated.

FIG. 10 is a schematic diagram of the concept of smoothing the filling surface of the present invention. Spraying is performed in a constant state by a particle dispersing device to form a mortar-shaped filling surface S1, and then a second mortar-shaped filling surface S2 having a reduced mortar-like size is formed inside the mortar-shaped filling surface S1. Then, a third mortar-shaped filling surface S3 having a reduced size is formed inside the second mortar-shaped filling surface S2. Here, three filling surfaces are shown, but in practice, smoothing of the filling surface can be easily realized by finer stepwise or continuous control. For example, when a filling surface having irregularities as shown in FIG. 11 is formed, an inclined portion is provided at the outer peripheral portion of the spraying region, so that the portion must be taken into consideration, and smoothing is difficult. In consideration of the controllability for smoothing the filling surface, a mortar-shaped filling surface S formed by performing spraying in a constant state in a range of the height at which the particles are filled in the filling container.
It intends line smoothing filling surface 1 shaped as a 2 ≧ h (edge) / h (ct) ≧ 1. Mortar-shaped filling surface S to be formed
If the shape of 1 is out of this range, it becomes difficult to smooth the filling surface. In particular, if h (edge) / h (ct) <1, it becomes almost impossible to smooth the filling surface. Also, h (e
dge) / h (ct) = 1, h
(Edge) / h (ct) <1 is conceivable, so if possible, 2 ≧ h (edge) / h (ct)> 1
It is preferable to carry out in. That is, the shape of the filling surface formed by spraying is 2 ≧ h (edge) / h (ct) ≧
The smoothing of the filling surface is performed while fluctuating between 1.

As parameters for changing the spraying conditions of the particle spraying apparatus, the number of rotations of the rotating disk is adjusted in the spraying apparatus shown in FIG. 5, and the number of rotations of the rotating blades is adjusted in the spraying apparatus shown in FIGS. In the spraying apparatus of FIG. 9, the spray radius and the spray amount can be changed by adjusting the rotation speed of the rotating disk. In addition, the rotating disk (blade) itself can be changed stepwise to one having a different diameter. The amount of particles supplied to the rotating disk (blades) can also be adjusted stepwise. The parameter is changed and smoothing is performed while the spraying state is recognized on the display device by the filling monitor. Further, in the conventional particle dispersing apparatus shown in FIGS. 5 and 6 to 8, the value of h (edge) / h (ct) greatly varies depending on the height of the filling surface. The parameters such as the number of revolutions and the amount of supplied particles are changed so as to be in an appropriate range.

In connection with the spraying device shown in FIG. 9, a supplementary explanation will be given on the shape of the rotating disk and the slit. As shown in FIG. 12, the rotating disk is assumed to be a half of a uniaxial spheroid. When the rotating disk is rotating at an angular velocity ω, the mass point m cast therein moves to a line with a radius r by centrifugal force and is balanced. The radius r can be represented by Equation 4.

[0031]

(Equation 4)

Here, r is considered to be the farthest position of the particle in the rotating disk at the angular velocity ω. FIG. 13 (a) shows the horizontal transfer of particles scattered from the slit located r from the center of the rotating disk, and the distance of the particles emitted at a linear velocity rω from the rotation center after t seconds. Is represented by Expression 5.

[0033]

(Equation 5)

Here, by substituting r in Equation 4, Equation 6 is obtained.
Becomes

[0035]

(Equation 6)

By the way, as shown in FIG. 13B, the time t at which the particles discharged to the filling surface having the height h reach is expressed by the following equation (7).

[0037]

(Equation 7)

By substituting this into Equation 6, the following Equation 8 is obtained.

[0039]

(Equation 8)

The dispersion range of the particles at the angular velocity ω is 0 to R
It can be seen that it is.

The slit on the rotating disk is required to have a condition that the particles immediately after being sprayed have an r ² distribution. It has been confirmed by particle scattering experiments that the conductance is constant regardless of the hole position (distance from the center of rotation) on the disk. Based on this, the shape of the slit on the rotating disk will be considered. In order to simplify the idea, it is assumed that the particles that have dropped to r ₀ are immediately given the angular velocity ω and move instantaneously to the balance point r of the mass point. The particles are continuously supplied to the hatched area in the center of FIG. 14 and move to the point r. By the way, as shown in FIG. 15, particles coming out of holes at radii r, 2r, and 3r are generally

[0042]

(Equation 9)

It falls to the position d _x ωt according to the above. However,
t is a value obtained by Expression 7. Here, FIG.
In (a) and (b), particles in the fan-shaped oblique line portion are scattered from the slit A at the position of the radius r, and the scatter range is the A region on the scatter surface. D of area A
_x is R, and this area S _A is

[0044]

(Equation 10)

Is as follows. Next, assuming that the particles in the fan-shaped oblique line portion are scattered from the slit B (2r), the scatter area is an annular B region on the scatter surface. Since d _x of the B region is 2R, the area S _{B of} this region is expressed as follows.

[0046]

[Equation 11]

However, the amount of particles coming out of the slit A and the amount of particles coming out of the slit B are the amounts supplied in the fan-shaped hatched portion, and are the same. Therefore, it can be seen that the slit B at the position 2r needs to be out of phase with the slit A and have a large S _B / S _A opening angle. Ideally

[0048]

(Equation 12)

The series solution is as follows. The meaning that the spatial distribution of the particles immediately after the dispersion is the r ² distribution indicates the first term shown in Expressions 11 and 12.

Assuming that all of the particles supplied from the respective particle supply units in FIG. 17 come out of the corresponding slits, the ideal slit shape curve is a series curve shown in equations (11) and (12). If this is simplified and the second term is ignored, a square curve with respect to r is obtained.

It can be seen that the condition under which no particles remain on the disk is that the end point E of the No. 1 slit and the start point S of the No. 2 slit shown in FIG. 18 overlap. Further, the value of the overlap limit r needs to be a balance point of the mass point at the minimum rotation speed at the time of dispersing particles. Further, unless the sum of the conductances of the slits in the range of 0 <r _x ≦ r is larger than the conductance of the orifice, particles will accumulate in the rotating disk. These are the basic requirements for the slit shape. After that, the motion of the particles sliding in the rotating disk should be examined, and this requirement should be superimposed on the result. FIG. 19 shows an example of calculation results of the slit shape.

Next, it is necessary that the rotating disk base line is a curve that coincides with the transport curve of the particles moving in the disk.
Consider the formula of this curve. Now, a rotating disk (a = b = c) having a radius a is rotating at an angular velocity ω. Consider the trajectory of one particle that has dropped from the orifice at point A that is r ₀ away from the rotation axis. Here, the friction coefficient (dynamic friction coefficient) between the particle and the rotating disk is constant, and the angular velocity of the rotational motion of the particle in the initial state is zero. When the particle and the rotating disk contacts subjected to centrifugal force corresponding to r ₀ position at that moment. The centrifugal force is given by the following equation (13).

[0053]

(Equation 13)

When the particles have the same angular velocity as the disk due to perfect friction, υ ₁ = ωr _0. However, since there is a loss in the transmission of energy due to friction, considering the energy transmission coefficient α, Is represented by

[0055]

[Equation 14]

That is, the centrifugal force f ₀ is expressed by the following equation (15).

[0057]

(Equation 15)

The balance point of the mass point on the rotating disk of a = b = c is expressed by the following equation (16).

[0059]

(Equation 16)

As a result of the above consideration, the relative motion between the particle and the rotating disk can be expressed by Expression 17 in a polar coordinate system which projects a uniaxial spheroidal disk as shown in FIG.

[0061]

[Equation 17]

The rotation speed of the rotating disk is actually changed according to the filling height, and the rotating speed m in the steady state of the rotating disk here is the rotating speed used constantly. B is the angle at which the particles dropped from the hopper are moved by the rotating disk until the particles rotate to the same rotational speed as the rotating disk, and can be obtained by calculation.

In this manner, the locus of movement of the particle which has fallen to the center of the uniaxial spheroidal disk while receiving the rotational force from the disk and moving until the particle coincides with the rotation speed of the disk is expressed by the following function in the above polar coordinate system. Can be.

[0064]

(Equation 18)

The trajectory function in which the delay angle in the rotational direction with respect to the moving distance in the radial direction from the center of the disk coincides with the required amount of particles to be scattered at the radial position is represented by the following function in the above polar coordinate system. It can be a trajectory represented.

[0066]

[Equation 19]

The function of the trajectory in which the delay angle in the rotational direction with respect to the moving distance in the radial direction from the center of the disk coincides with the required amount of the particles to be scattered at the radial position is represented by the following function in the above polar coordinate system. Trajectory.

[0068]

(Equation 20)

By expressing the shape of the slit of the uniaxial spheroidal disk by the above-mentioned equations (18) and (19) or equations (18) and (20), the shape of the mortar-shaped filling surface formed when spraying is performed in a fixed state is determined. 2 ≧ h (edge) / h (ct) ≧ 1
A particle filling device that can be easily controlled within the range described above can be realized.

[0070]

【Example】

(Example 1) Disk a = 20 cm, c = 12 cm, number of slits = 4, slit width = 8 mm, orifice diameter = 9
Using a packing device of 5 mmφ, equipped with a particle distribution device of the type of FIG. 9 (slit shape determined on the basis of the above-mentioned idea, FIG. 21), a height of 1.
Attach the filling device at 4m, 1.6m, 0.6m,
0.5 to 0.5 mm from the filling device at each height
1.5 mm, 3 to 5 mm long cylindrical ceramic catalyst particles (cross-sectional area: 0.0152 cm ^{2 to} 0.0783 c
m ² ) is the number of revolutions of the rotating disk whose maximum scattering distance exactly matches the wall surface of the packed tower.
The catalyst was sprayed at a speed of 5 ton / min, and the catalyst spraying characteristics of the disk were determined from the shape of the packing surface at that time. Table 1 shows the scattering amount of the catalyst particles in each section with respect to the fourth section for each height. In this section, the center of the packed tower is the 0th section, the wall of the packed tower is the 5th section, and the first section, the 2nd section, the 3rd section, and the 4th section are equally spaced from the center of the packed tower.
This is represented as a division (FIG. 22). In addition, the height is expressed based on the filling device as 0 m. As shown in Table 1, the shape h (edge) / h (ct) of the mortar-shaped filling surface formed when spraying is performed in a constant state.
Is controlled in the range of 1-2.

[0071]

[Table 1]

FIG. 22 shows a simplified control pattern of the catalyst dispersion when the catalyst is filled from -3.6 m to -1.5 m based on the experimental results in Table 1. The method of simplification in FIG. 22 is from -3.6 m to -3.0.
Uncontrolled spraying (only the number of revolutions is controlled so that the distance to the wall of the packed tower always becomes the maximum scattering distance) is performed with the characteristics according to the data of -3.60 m in Table 1 up to m. Perform a smoothing operation. Then, from -3.0m to -2.0
Uncontrolled spraying is performed with data of -2.40 m in Table 1 up to m, and a smoothing operation of the filling surface is performed at -2.0 m. Similarly, it shows the flattening operation (scattering distance and time ratio) obtained at each height when the flattening operation is performed even at the time of -1.0 m.

From the result shown in FIG. 22, for example, -2.0 m
In, for the time required for filling from -3.0 m to -2.0 m (100%), spraying was performed for 2% of the time so that the 1.2th division had the maximum scattering distance, and thereafter, It shows that an approximately flat filling surface can be obtained by performing the spraying for 5.5% of the time so that the 3.0 section becomes the maximum scattering distance. If the scatter range and time obtained in this way are more finely dispersed, for example, if the unit time is 5 minutes, the scatter at which the fifth section (wall surface) has the maximum scatter distance in the filling between -3 m and -2 m. For 5 minutes (300 seconds (1
00%)), after that, the spraying was performed for 6 seconds (2%) at which the 1.2th section had the maximum distance, and the spraying was further performed at 17 seconds (5.5%) at which the 3.0th section had the maximum scattering distance. After performing, the spraying pattern in which the fifth section (wall surface) returns to the spraying with the maximum scattering distance is repeated. As a result, a surface smoother than the filling surface shown in FIG. 22 is obtained. Therefore, the shape of the filling surface varies in the range of 2 ≧ h (edge) / h (ct) ≧ 1.

Example 2 Using the filling device of Example 1,
Tower diameter 4.1m, height 15m, three-layer structure (each layer 3.6m)
Was spray-filled with the catalyst particles of Example 1 (spraying range; -3.6 m to -2.5 m). In addition, a supporting catalyst is sprayed in advance on the bottom of the indirect deflow device, and its filling surface is leveled. Further, the surface on which the catalyst particles were deposited was scanned with a laser beam, and the state of the packed surface was measured. The number of measurement points was 100, and the measurement interval was once every 30 seconds.
The measurement was based on semiconductor laser beam scanning and triangulation of the filling surface with a CCD camera. Laser beam is 35m
A W semiconductor laser was used. The camera has a focal length of 35
mm monochrome CCD camera of 380,000 pixels was used (minimum subject illuminance: 0.2 Lux). 512x
A 512 pixel image processor was used. (Note that the coordinates of the laser spot were determined with a recognition accuracy of 0.1 pixel unit.)

The basic rotation speed of the filling device (the rotation speed at which the maximum scattering distance at the height of the filling surface is the wall surface) was controlled as shown in Table 2 according to the height of the filling surface. The filling surface height in Table 2 represents the distance from the position of the filling device to the filling surface, and shows the relationship between the maximum scattering distance, the filling surface height, and the rotation speed.

[0076]

[Table 2]

In addition, the filling surface flattening operation is performed with a unit time of 5 minutes, based on the value obtained in the first embodiment, and further measured by the filling monitor and updated every 30 seconds.
The amount of the filling surface was adjusted while checking the height of the filling surface at the measurement point. FIG. 23 shows an example of the filling result. A solid line indicates a measurement result of the filling monitoring monitor which is one section of the filling surface extracted with time (extracted at intervals of about 15 minutes from a result of continuous sampling). Measurement results), and the dotted line is the actual measurement value that the operator confirmed on the tape measure (except for the data at the end of filling and at the beginning of filling, the solid line and the dotted line do not show the values measured at the same time, so Is shifted.) As shown in FIG. 23, it was confirmed that the height difference of the filling surface was reduced to about 5 cm by this method.

[0078]

According to the present invention, in a constant state (for example, in an uncontrolled state)
The size of the mortar is determined using a particle-dispersing device having a parameter capable of forming a mortar-shaped filling surface and controlling the mortar-shaped size when spraying and a particle-filling device having a filling monitoring monitor. By gradually reducing the size, smoothing of the particle-filled surface can be easily realized.

[Brief description of the drawings]

FIG. 1 (a) is a partial cross-sectional view from the front direction of an example of a particle filling device used in the present invention,
FIG. 1B is an explanatory view showing a state of scanning the filling surface by the scanning laser beam.

FIG. 2 is an explanatory view showing how a laser generation and scanning device and an imaging device are attached to a container wall.

FIG. 3 shows an example of a laser and camera arrangement of a 4 camera × 2 laser system, and a -5 m field of view and a -10 m field of view are indicated by dotted lines.

FIG. 4 is a basic screen configuration diagram of a filling surface monitoring monitor.

FIG. 5 shows an example of a filling device that can be used in the present invention, and (a)
Shows a side view and (b) shows a bottom slit.

FIG. 6 is a conceptual diagram of a Densi Cat type catalyst spraying device.

FIG. 7 is a conceptual diagram of a UOP type catalyst dispersion device,
(A) is a front sectional view, and (b) is a top view of the blade.

FIG. 8 is a conceptual diagram of a COP type catalyst spraying apparatus,
(A) is a front sectional view, and (b) is a top view of the blade.

FIG. 9 is a partial cross-sectional view from the front of another example of the particle filling apparatus used in the present invention.

FIG. 10 (a) is a schematic diagram of the concept of smoothing the filling surface of the present invention, and FIG. 10 (b) is an explanatory diagram showing the definitions of h (ct) and h (edge) in the present invention.

FIG. 11 shows an example of a filling surface that is difficult to smooth.

FIG. 12 is an explanatory diagram illustrating mass points of a tachometer.

FIGS. 13A and 13B are explanatory diagrams showing a particle scattering state, wherein FIG. 13A shows horizontal transfer of particles and FIG. 13B shows vertical transfer of particles.

FIG. 14 is an explanatory diagram showing a relationship between a particle supply area and conveyance.

FIG. 15 is an explanatory diagram illustrating a particle scattering range.

FIGS. 16A and 16B are explanatory diagrams showing a relationship with a slit spray surface, wherein FIG. 16A shows a rotating disk and FIG. 16B shows a spray surface.

FIG. 17 is an explanatory diagram illustrating a required slit opening angle.

FIG. 18 is an idealized slit curve showing that the end point E of the No. 1 slit and the start point S of the No. 2 slit overlap.

FIG. 19 shows a calculation result example of a slit shape.

FIG. 20 shows a polar coordinate system obtained by projecting a rotating disk.

FIG. 21 is a schematic diagram in a polar coordinate system of a slit shape of a rotating disk in the embodiment.

FIG. 22 is a graph showing an aspect of deposition of a filling surface in connection with Example 1.

FIG. 23 is a graph showing a filling result in connection with Example 2, wherein a solid line is a measurement result of a filling monitoring monitor which extracts one section of the filling surface with time, and a dotted line is a worker confirms with a tape measure. This is the measured value.

[Explanation of symbols]

 C catalyst particles S catalyst particle filling surface 1 reaction vessel 2 filling device 3 spraying device 4 filling monitoring monitor 5 laser generation and scanning device 6 scanning laser beam 7 laser source 8 laser scanner 9 imaging device 10 camera 11 computer 13 CRT 15 signal line 16 Air line 17, 19 Dustproof cover 18, 20 Fixture 21 Side slit 22 Bottom 23 Lower slit 24 Rotating disk 25 Door 31 Hanging tool 32 Outer cover 33 Hopper 34 Rotating shaft 35 Motor 36 Disk 37 Slit 38 Supporting means 39 Orifice 40 Hose 41 Dispersion plate 42 Outer sheath 43 Actuator 44 Fixing leg

Claims (10)

(57) [Claims] 1. A particle dispersing device having a parameter capable of forming a mortar-shaped filling surface and controlling the size of a mortar when spraying in a constant state, and continuously filling the entire filling surface. It is a method of smoothing a particle filling surface in a particle filling device comprising a filling monitoring monitor that can be grasped, and while the filling monitoring monitor continuously grasps the state of formation of the filling surface, the particle dispersion device keeps a constant. Forming a mortar-shaped filling surface by performing spraying in the state of, and controlling the parameters of the particle scattering device intermittently or continuously to gradually reduce the mortar-shaped size inside the mortar-shaped filling surface. The filling surfaces are sequentially deposited at predetermined intervals or continuously, in which case the filling container is filled with particles.
In the range of height, the particle
The center of the mortar-shaped filling surface formed when spraying
The height (h (ct)) and the height of the surrounding filling surface (h (edg)
e)) is expressed as (h (edge) / h (ct)).
When the mortar is formed by spraying in a certain state
The shape of the filling surface is 2 ≧ h (edge) / h (ct) ≧ 1
To the smoothing method of particle packing surface in particle packing apparatus characterized by smoothing the packing surface. 2. The method of claim 1, wherein the step of forming the smooth filling surface is repeated. 3. A mortar-shaped filling surface can be formed when dispersing the particles in the filling container with the maximum scattering distance of the particles being the wall surface of the filling container at its filling surface. 2. The method of claim 1, wherein the apparatus is a particle scattering device having a parameter whose size can be controlled. 4. A particle dispersing device comprising a side slit with an adjustable door and a lower slit on the bottom surface,
Rotating disk is attached to the bottom surface, claim, characterized in that it is of the type capable of controlling the distribution state by adjusting the rotational speed of the opening and the rotary disc side and lower slits 1-3 The method of any one of the preceding claims. 5. An apparatus for dispersing particles, an outer cover, a hopper supported by the outer cover inside the outer cover and having an open lower end, a rotation supported by the hopper and extending outwardly from the opening through the center of the hopper. A motor having a shaft, and a uniaxial spheroid disk fixed to a lower end of the motor rotation shaft and receiving particles falling from the hopper, wherein a slit for discharging particles is formed in the uniaxial spheroid disk. The movement trajectory of the particles in which the shape of the slit falls from the hopper to the central area of the uniaxial spheroidal disk until the particles receive the rotational force from the disk and move until the number of rotations of the disk coincides with each other, and from the center of the disk to the radial direction. The delay angle in the rotation direction with respect to the distance traveled is expressed as the sum of the function of the trajectory that matches the required amount of particles sprayed from its radial position toward the filling surface. 4. The method according to claim 1 , wherein the method is of the type: 6. The movement trajectory of a catalyst, which is moved until particles falling at the center of a uniaxial spheroidal disk receive rotational force from the disk and reach the rotation speed of the disk, are expressed by the following function. The method of claim 5 . (Equation 1) 7. A function of a trajectory in which a delay angle in a rotational direction with respect to a moving distance in a radial direction from a center of a disk coincides with a required amount of catalyst to be scattered at the radial position is represented by the following function. The method of claim 5 , wherein (Equation 2) 8. A function of a trajectory in which a delay angle in a rotational direction with respect to a moving distance in a radial direction from a center of a disk coincides with a required amount of catalyst dispersed at the radial position is represented by the following function. The method of claim 5 , wherein (Equation 3) 9. A filling monitoring monitor, which is attached to a container for filling particles at a level higher than the particle filling height, is selected according to a target accuracy not less than a cross-sectional area of the particles for scanning a particle deposition surface with laser light. Device for generating and scanning a laser beam having a laser beam diameter to be measured and an imaging device for detecting laser reflected light from a scanning point, and the position of the specific scanning point during measurement, and the position of the laser beam generating and scanning device And a display device for calculating a depth of a scanning point from the position of the imaging device by trigonometry, and a display device for displaying data including a deposition surface depth distribution. Method 1 . Any one of the methods of claims 1-9, characterized in that 10. A particle is the catalyst.