CN107870138B - Device for on-line detection of particle properties in fluidized bed granulation process - Google Patents
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- 239000008187 granular material Substances 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 7
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- 238000009477 fluid bed granulation Methods 0.000 claims 8
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The device for on-line detection of particle properties in the fluidized bed granulation process is provided with a sealed shell, a sample acquisition mechanism, a first visual detection unit, a second visual detection unit and an image processing system; the first visual detection unit comprises a first camera, a circular tray and a pressure sensor; the image processing system obtains particle size information from the falling image of the sample, and obtains the angle of repose from the sample deposit image
(ii) a The second visual detection unit comprises a measuring cylinder, a measuring cylinder fixing plate, a light source, a vibration table and a second camera, and the image processing system obtains the loose density of the particles from the sample image in the measuring cylinder before the vibration table is started
Obtaining the tap density of the particles from an image of the sample in the cylinder during vibration of the vibration table
. The invention has the advantages of on-line detection of the particle size distribution, the angle of repose, the apparent density, the tap density, the porosity and the Haosner ratio of the particles in the granulation process of the fluidized bed.
Description
Technical Field
A device that is used for granule nature on-line measuring in fluidized bed pelletization process.
Background
The granulation fluidized bed completes granulation, coating and drying in the pharmaceutical process in one step, and is widely used in the pharmaceutical production link.
The particle diameter range of the fluidized bed not only affects the next process flow, but also affects the final medicine quality. The operation parameters of the existing granulation fluidized bed are fixed during production, the batches and the environment of raw materials change along with time, and the operation parameters cannot change along with the changes, so that the obtained medicine has poor quality consistency and even is unqualified. The particle diameter is detected on line in real time, and the operation parameters can be changed according to the changes, so that the particle diameter is distributed in an expected range, the granulating process can be monitored, and the quality of the medicine can be controlled, so that the on-line detection of the particle diameter in the fluidized bed granulating process is necessary.
Quality inspection is always an important step for ensuring the qualified quality of medicines. For fluidized bed products, the quality control generally includes particle size distribution, particle size, moisture content, angle of repose, apparent density, tap density, porosity, hausner ratio, and the like.
Chinese patent application CN201510638050.7 discloses a detection device for on-line detecting particle diameter distribution in a granulation fluidized bed, which is installed outside the reaction chamber of the fluidized bed; the detection device is provided with a sealed shell, a sampling mechanism which can extend into the fluidized bed reaction chamber to take out a sample is arranged in the shell, the sampling mechanism is positioned at a sampling station when extending into the fluidized bed reaction chamber, the sampling mechanism is positioned at a dispersing station when dropping the sample after exiting from the fluidized bed reaction chamber, and the sampling mechanism reciprocates between the sampling station and the dispersing station; the sampling mechanism is matched with the wall of the fluidized bed reaction chamber in a sealing way; a visual detection mechanism is arranged in the shell and comprises a light source and a camera, and the camera shoots the falling process of the sample; a recovery mechanism for collecting samples is arranged in the shell. The disadvantages of such a detection device are: the particle size distribution of the particles in the fluidized bed can be detected only on line, and parameters such as the angle of repose, the apparent density, the tap density and the like cannot be detected.
The quality inspection method of the particles prepared by the fluidized bed at present is that after granulation is finished, a final product is sampled, the particle size distribution of the particles is inspected by adopting a screening method or a particle sizer, the particle size is calculated, the angle of repose of the particles is inspected by adopting an injection method, the loose packing density of the particles is inspected by adopting a funnel method, the tap density of the particles is inspected by adopting a tap method, after the parameters are obtained, the porosity and the Haosner ratio of the particles are calculated according to a formula, and then the quality of the particles is judged. The detection method has simple equipment and low cost, but is complex to operate, the properties of the particles need to be separately measured by a plurality of different instruments, the characteristics of the particles are easy to change in the transferring process, the accuracy of the measurement result is poor, and the proficiency of operators can influence the measurement result; meanwhile, the method belongs to an off-line detection mode, has great hysteresis and can not meet the requirement of industrial production on-line monitoring.
Disclosure of Invention
The invention aims to provide a detection device capable of detecting the particle size distribution, the angle of repose, the apparent density, the tap density, the porosity and the hausner ratio of particles in a fluidized bed granulation process on line.
The detection device is arranged outside a reaction chamber of the fluidized bed, and is provided with a sealed shell, a sample acquisition mechanism capable of taking out a sample from the reaction chamber, and a first visual detection unit which is positioned in the shell and shoots the falling process of the taken sample in the shell;
the method is characterized in that: a second visual detection unit for detecting the apparent density and the tap density of the sample is arranged in the shell, the sample is transferred from the first visual detection unit to the second visual detection unit by the sample transfer mechanism, and image information obtained by the first visual detection unit and the second visual detection unit is input into the image processing system;
the first visual detection unit comprises a first camera, a circular tray and a pressure sensor arranged below the circular tray; the circular tray receives a sample falling from the sample collecting mechanism, the first camera shoots the falling process of the sample and an image of a sample deposit on the circular tray, and the image processing system obtains particle size information from the falling image of the sample and obtains an angle of repose from the image of the sample deposit
；
The sample transfer mechanism comprises a rotary motor and a collection funnel, the rotary motor is fixedly connected with a supporting shaft of the circular tray, the supporting shaft is fixed at the lower end of the circular tray and is positioned on a circular central axis of the circular tray, when the rotary motor is positioned at a first position, the circular tray is upright to receive a falling sample, and when the rotary motor is positioned at a second position, the circular tray is inclined in a vibration mode to pour all the samples on the circular tray into the collection funnel;
the second visual detection unit comprises a measuring cylinder for receiving the materials from the collecting funnel, a measuring cylinder fixing plate, a light source, a vibration table and a second camera, the measuring cylinder is fixed on the measuring cylinder fixing plate, the measuring cylinder fixing plate is arranged on the vibration table, and the second camera and the light source shoot a sample image in the measuring cylinder; the image processing system obtains the loose packing density of the particles from the sample image in the measuring cylinder before the vibration table is started
Obtaining the tap density of the particles from the sample image in the measuring cylinder after the vibration of the vibration table
. To obtain apparent density
And tap density
Then according to the formula
Calculating to obtain the porosity of the particles
，
The hausner ratio HF is calculated.
Further, first visual inspection unit contains a plurality of level mirrors and a plurality of area source, and level mirror and area source interval distribution enclose into the regular polygon region that has the breach with the area source, and first camera sets up in this breach department, and circular tray is located this regular polygon region.
Furthermore, the circular tray is positioned in the center of the regular polygon area, and a sample blanking port of the sample collecting mechanism is aligned to the circle center of the circular tray; the sample deposit image comprises a direct image of the deposit on the circular tray and indirect images of the deposit on the circular tray in each plane mirror; the image processing system acquires height data of the deposit in each image, calculates the angle of repose using the average height as the height H for calculation
And R is the radius of the circular tray. The circular tray is positioned in the center of the regular polygon area, the sample blanking port of the sample collecting mechanism is aligned with the circle center of the circular tray, so that a sample can be dropped on the circular tray to gradually form conical deposits, and the inclination angle of the conical deposits is the angle of repose.
Further, the first camera shoots an image of a deposit on the circular tray in real time, and when the height of a cone of the image of the deposit is not changed, the sample collection mechanism stops sampling; after the sample collection mechanism stops sampling, the pressure sensor obtains the quality of the sample particles on the circular tray
Apparent density of
，
A scale for locating the sample particles before vibration, shot by the second camera, in the measuring cylinder; tap density
，
The vibrated sample particles photographed by the second camera are located on a scale in the graduated cylinder.
Furthermore, in the first visual detection unit, the adjacent surface light sources and the plane mirrors form an included angle of 120 degrees, the number of the surface light sources is 3, and the number of the plane mirrors is 2; the surface light source and the plane mirror are enclosed into a regular hexagon area with a gap.
Furthermore, the collecting funnel consists of a first funnel and a second funnel, the second funnel receives the transfer blanking of the circular tray, and the first funnel receives the overflow blanking when the circular tray is in an upright state; the second funnel is communicated with the first funnel, the outlet of the second funnel is aligned in the measuring cylinder, and the outlet of the first funnel is aligned with the first waste sample collecting box.
In the vibration process of the vibration table, the second camera samples the image of the measuring cylinder at fixed intervals until the volume difference value of the samples in the previous and next two times is less than 2mL, and the image processing system reads the volume scale of the particles in the measuring cylinder
。
Further, the measuring cylinder fixing plate is connected with a discharging motor, and the discharging motor is fixed on the table top of the vibration table; when the opening of the measuring cylinder is vertically upward, the discharging motor is positioned at a visual detection position; when the opening of the measuring cylinder is vertically downward, the discharging motor reaches the discharging position; in the discharge position, the sample in the measuring cylinder falls into the second waste sample collecting box. The two sides of the measuring cylinder fixing plate are respectively provided with a slot, and the base of the measuring cylinder is inserted into the slots and is in interference fit with the slots. The first waste sample collection box and the second waste sample collection box are both placed on the bottom plate of the shell.
Further, a disc is arranged on the vibration table, a second rotating motor is arranged on the disc, the second rotating motor is an outer rotor motor, an outer rotor of the second rotating motor is fixedly connected with the disc, and the inner stator is hollow; an output shaft of the vibrating table penetrates through the disc and the second rotating motor, a buckle is arranged at the top end of the output shaft, and the second rotating motor and the disc are tightly abutted to the vibrating table through the buckle; and two measuring cylinders and measuring cylinder fixing plates are arranged on the disc, each measuring cylinder fixing plate is connected with a respective unloading motor, an opening of the measuring cylinder aligned with the second hopper is upward and positioned at a detection station, the other measuring cylinder is positioned at an unloading station, and the second waste sample collecting box is positioned below the unloading station.
Furthermore, the sample collecting mechanism is positioned outside the shell and mainly comprises a collecting sleeve, a piston rod, a collecting piston at the end of the piston rod and a sampling pushing piece, wherein the sampling piston is in sealing fit with the sampling sleeve; when the sampling mechanism stops sampling, the sampling piston isolates the inlet and the outlet of the sampling sleeve.
Furthermore, a speed reducing conduit is arranged between the sampling sleeve and the shell, the speed reducing conduit is a bent pipe, an inlet of the speed reducing conduit is communicated with an outlet of the sampling sleeve, an outlet of the speed reducing conduit is communicated with an inner cavity of the shell, an outlet of the speed reducing conduit is used as a sample blanking port of the sample collecting mechanism, and an inlet of the speed reducing conduit is higher than an outlet of the speed reducing conduit.
The invention has the advantages that: 1. the method has the advantages that multiple attributes (particle size distribution, angle of repose, loose packed density, tap density, porosity and Hausner ratio) of the granules in the fluidized bed granulation process are monitored on line, various properties of the granules in the granulation process are reflected comprehensively, the monitoring capability of the pharmaceutical process is improved, and the understanding of the pharmaceutical process and the optimization of the pharmaceutical process are facilitated.
2. The automatic detection equipment improves the detection environment, reduces the detection speed of the detection equipment and the requirement of additionally cleaning accessories, and avoids the defects of off-line detection, such as cross contamination, large errors of manual operation and the like.
3. Meanwhile, the multi-attribute of the particles (particle size distribution, angle of repose, apparent density, tap density, porosity and Hausner ratio) is inspected, so that the inspection time is greatly saved, and the requirement of automatic online monitoring of industrial production is met.
4. In the test, the particle attributes are obtained by processing through an image method, the accuracy of the image detection method is high, and the human error of the traditional off-line detection method is avoided to the maximum extent.
Drawings
FIG. 1 is a schematic view showing the appearance of the present invention when installed in a fluidized-bed reaction chamber.
Fig. 2 is a schematic diagram of the overall structure of the device.
Fig. 3 is a partial structure schematic diagram of the device.
Fig. 4 is a schematic illustration of visual measurements of particle size and angle of repose.
Fig. 5 is a schematic diagram of a sample transfer process.
FIG. 6 is a schematic diagram of a bulk density and tap density measurement structure.
Fig. 7 is a schematic view of the structure of the vibration table.
In the figure:
the device comprises a detection device A, 1, a reaction chamber, 2, a sampling sleeve, 3, a piston rod, 4, a sampling pushing part, 5, a speed reduction guide pipe, 6, a plane mirror, 7, a surface light source of a first visual detection mechanism, 8, a first camera, 9, a rotating motor, 10, a first funnel, 11, a second camera, 12, a measuring cylinder, 13, a disk, 14, a measuring cylinder fixing plate, 15, a first waste sample collection box, 16, a discharging motor, 17, a second funnel, 18, a circular tray, 19, a vibration table, 20, a second waste sample collection box, 21, a surface light source of a second visual detection mechanism, 22, sample particles in the falling process, 23, a pressure sensor, 24, a second rotating motor, 25 and a buckle.
Detailed Description
As shown in fig. 1, the on-line detecting device for detecting the properties of granules in the fluidized bed granulation process is characterized in that a detecting device a is arranged outside a fluidized bed reaction chamber 1; the detection device A has a sealed housing and a sample collection mechanism capable of taking a sample from the reaction chamber 1.
As shown in fig. 2, a first visual detection unit for shooting the falling process of the taken sample in the shell is arranged in the shell; the shell is internally provided with a second visual detection unit for detecting the loose density and the tap density of the sample, the sample is transferred from the first visual detection unit to the second visual detection unit by the sample transfer mechanism, and image information obtained by the first visual detection unit and the second visual detection unit is input into the image processing system.
As shown in fig. 2, the sample collecting mechanism mainly comprises a sampling sleeve 2, a piston rod 3, a sampling piston at the head end of the piston rod 3 and a sampling pushing member 4; a sampling channel is arranged on the fluidized bed reaction chamber 1 and is communicated with the inner cavity of the sampling sleeve 2; the sampling piston is in sealing fit with the sampling sleeve 2, and the piston rod 3 is connected with the sampling pushing piece 4; the sampling sleeve 2 is provided with an inlet communicated with the reaction chamber 1 and an outlet communicated with the shell, and when the sample collecting mechanism is in a sampling state, the inlet and the outlet of the sampling sleeve 2 are communicated; when the sampling mechanism stops sampling, the sampling piston isolates the inlet and the outlet of the sampling sleeve 2.
As shown in fig. 2, a deceleration conduit 5 is arranged between the sampling sleeve 2 and the housing, the deceleration conduit 5 is a bent pipe, an inlet of the deceleration conduit 5 is communicated with an outlet of the sampling sleeve 2, an outlet of the deceleration conduit 5 is communicated with the inner cavity of the housing, an outlet of the deceleration conduit 5 is used as a sample dropping port of the sample collecting mechanism, and an inlet of the deceleration conduit 5 is higher than an outlet of the deceleration conduit 5.
A local sample in the fluidized bed reaction chamber 1 is taken out by using a sample collecting mechanism, particles moving inside the fluidized bed are led out to the outside of the fluidized bed reaction chamber 1, the sample falls in a shell, and then the falling particles are detected by a visual detection system. The deceleration guide pipe 5 is designed to be bent, so that the movement speed of particles can be slowed down, a visual system can capture particle images conveniently, and particle size detection is carried out.
The first visual detection unit comprises a plurality of plane mirrors 6, a plurality of surface light sources 7, a first camera 8, a circular tray 18 and a pressure sensor 23 arranged on the circular tray 18; the plane mirror 6 and the surface light source 7 are distributed at intervals, the plane mirror 6 and the surface light source 7 enclose a regular polygon area with a gap, the first camera 8 is arranged at the gap, and the circular tray 18 is positioned in the regular polygon area; the round tray 18 receives the sample falling from the sample collecting mechanism, the first camera 8 shoots the falling process of the sample and the image of the sample deposit on the round tray 18, the image processing system obtains the particle size information from the falling image of the sample and the angle of repose from the image of the sample deposit
。
The circular tray 18 is located at the center of the regular polygon area, and the sample blanking port of the sample collection mechanism is aligned with the center of the circular tray 18. The sample particles taken out by the sample collection mechanism slowly fall on the circular tray 18, and the sample particles form a conical deposit on the circular tray 18, and at this time, the first camera 8 captures an image of the conical deposit to acquire the contour of the conical deposit.
The sample deposit image contains a direct image of the deposit on the circular tray 18 and an indirect image of the deposit on the circular tray 18 in each flat mirror 6; the image processing system acquires height data of the deposit in each image, calculates the angle of repose using the average height as the height H for calculation
And R is the radius of the circular tray 18. The circular tray 18 is positioned at the center of the regular polygon area, and the sample dropping opening of the sample collecting mechanism is aligned with the center of the circle of the circular tray 18, so that the sample drops on the circular tray 18 to gradually form a conical deposit, and the inclination angle of the conical deposit is the angle of repose.
The first camera 8 shoots an image of a deposit on the circular tray 18 in real time, and when the height of the image of the deposit is not changed, the sample collection mechanism stops sampling; after the sample collection mechanism stops sampling, the pressure sensor 23 obtains the quality of the sample particles on the circular tray 18
。
The falling speed of the particles in the detection device is lower than that in the fluidized bed reaction chamber 1, so that the camera lens is prevented from being polluted by the particles, and clear falling images of the particles can be shot by the camera, so that the distribution condition of the particle diameters of the particles can be accurately detected. The real-time detection of the particle size is placed outside the fluidized bed reaction chamber 1, the detection environment is improved, the detection speed of the detection equipment and the requirement for additionally cleaning accessories are reduced, the whole detection equipment can be transformed on the original equipment, the whole detection device is sealed, no external pollution is introduced to a detection sample, and the GMP production standard is met.
The first camera 8 is right opposite to the circular tray 18, and can collect images of particle falling processes and particle deposits on the circular tray 18 at the same time. A pressure sensor 23 is arranged below the circular tray 18 and has the function of measuring the quality of sample particles on the circular tray 18.
As shown in fig. 2 and 3, in the first visual inspection unit, the adjacent surface light sources 7 form an angle of 120 ° with the plane mirrors 6, there are 3 surface light sources 7, and there are 2 plane mirrors 6; the surface light source 7 and the plane mirror 6 enclose a regular hexagonal region having a notch, but the number of the surface light source 7 and the plane mirror 6 is not limited to the example of the present embodiment. The plane mirror 6 can image the particles falling in the air and the particle accumulation on the circular tray 18, can completely project the image of the sample, the first camera 8 can simultaneously acquire the images of the particles falling in the air and the particle accumulation in three directions, and the particle size distribution and the angle of repose information of the particles can be accurately and comprehensively acquired. The surface light source 7 can make the image collecting effect clearer as a backlight source.
The particles fall into the shooting range of the first camera 8 in the process of falling into the circular tray 18 from the deceleration guide pipe 5, the first camera 8 collects images of the falling particles, the image processing system obtains a direct image of the sample particles falling onto the circular tray 18 and indirect images in the two plane mirrors 6, denoising, graying and binaryzation preprocessing are carried out on the photos, calculation of particle size distribution of the particles is completed according to the pixel area of each particle image area, and the results are stored. And after the set detection effect is achieved, the visual system stops processing the particle size information in the picture.
The radius of the circular tray 18 is R, and the sample particles slowly fall on the circular tray 18 under the action of the deceleration guide 5 to form a conical accumulation, as shown in fig. 4 (b). The particle angle of repose is the maximum angle measured in a static state when the gravity and the friction force between particles reach equilibrium when the particles slide on the free inclined surface of the powder accumulation layer in the gravity field. When the accumulation state is unchanged, the excess particles slide down from the conical accumulation surface to the first hopper 10 directly below the circular tray 18, as shown in fig. 4 (a).
Simultaneously with the particle size distribution detection, the vision system acquires images of the conical deposit on the circular tray 18 and the indirect image of the conical deposit in the two flat mirrors 6 from the images, as shown in FIG. 4 (a). The method comprises the steps of conducting denoising, graying and binarization preprocessing on photographs of each angle (3 angles in the embodiment) of a deposit to obtain height data of a conical deposit, averaging the heights of the conical deposit in images of each direction (3 directions in the embodiment) to obtain a height H for calculation, and calculating the angle of repose of particles
. When the measured particle angle of repose is not changed, the accumulation is stable, the sampling of the sample acquisition mechanism is stopped, and the particles stop falling. The image processing system saves the stable particle angle of repose results. The pressure sensor 23 collects the mass data at this time, that is, the mass m of the particles0The vision system stops processing the information of the angle of repose of the particles in the picture.
After the first visual detection unit finishes particle size distribution and angle of repose measurement, the sample transfer mechanism sends the particles collected by the circular tray 18 into the second visual detection unit, and in order to prevent incomplete transfer, the rotating motor 9 enables the circular tray 18 to shake with fixed amplitude after inclining for a certain angle, and the sample is completely transferred to the second visual detection unit to measure loose density and tap density.
As shown in fig. 5, the sample transfer mechanism includes a first rotating motor 9 and a collecting funnel, the first rotating motor 9 is fixedly connected to a holding shaft of the circular tray 18, the holding shaft is fixed at the lower end of the circular tray 18 and is located on the circular central axis of the circular tray 18, when the first rotating motor 9 is in the first position state, the circular tray 18 is upright to receive the falling sample, when the first rotating motor 9 is in the second position state, the circular tray 18 is inclined and shakes with a fixed amplitude, and the sample thereon is poured into the collecting funnel.
As shown in fig. 5, the collecting funnel is composed of a first funnel 10 and a second funnel 17, the second funnel 17 receives the transfer blanking of the circular tray 18, and the first funnel 10 receives the overflow blanking when the circular tray 18 is in an upright state; the second funnel 17 is in communication with the first funnel 10, with the outlet of the second funnel 17 aligned with the measuring cylinder 12 and the outlet of the first funnel 10 aligned with the first waste collection box 15. The first hopper 10 and the second hopper 17 are provided with notches, and the notches of the two hoppers are bonded together, so that redundant powder on the circular tray 18 in a vertical state only falls on the first hopper 10, and particles only fall on the second hopper 17 during material transfer.
As shown in fig. 5, the first rotating motor 9 rotates the circular tray 18 clockwise by 90 degrees, and the particles on the circular tray 18 fall into the measuring cylinder 12 right below through the second hopper 17. While the first rotary motor 9 oscillates in a small range so that the sample on the circular tray 18 can fall down into the measuring cylinder 12 in its entirety. Then, the first rotating motor 9 drives the circular tray 18 to rotate 90 degrees counterclockwise, and the circular tray 18 is reset to prepare for the next detection of the particle size and the angle of repose.
As shown in fig. 5, the second visual inspection unit includes a measuring cylinder 12 receiving the incoming material from the collection funnel, a measuring cylinder fixing plate 14, a surface light source 21, a vibration table 19, and a second camera 11, the measuring cylinder 12 is fixed on the measuring cylinder fixing plate 14, the measuring cylinder fixing plate 14 is mounted on the vibration table 19, and the surface light source 21 is matched with the second camera 11 to photograph the sample image in the measuring cylinder 12; image processing System the apparent density of the particles is obtained from an image of the sample in the graduated cylinder 12 before the vibrating table 19 is activated
Obtaining the tap density of the particles from the sample image in the measuring cylinder 12 after the vibration by the vibration table 19
. To obtain apparent density
And tap density
Then, the porosity of the particles is calculated
Calculating to obtain the Haosner ratio
。
The volume of the conical stack should be less than the maximum volume of the measuring cylinder 12, and the properties of the different particles will vary, so that it is necessary to determine the diameter of the circular tray 18 with respect to a specific object.
After the measuring cylinder 12 collects the particles supplied by the circular tray 18, the second camera 11 acquires an image of the particles in the measuring cylinder 12, and the image processing system gives the particle volume V according to the position information of the sample surface and the scale1According toρ b =m0/V1Calculating the bulk density of the particles (ρ b ). After the bulk density of the particles is measured, the vibration table 19 starts to vibrate.
The vibration table starts to vibrate under the parameters that the amplitude is 3mm and the vibration frequency is 300 times/min, the second camera collects images of the measuring cylinder 12 at fixed intervals in the vibration process until the difference value of the sample volume is less than 2mL, and the image processing system reads the particle volume V2Calculating the particle tap density (ρ t ) I.e. byρt=m0/V2。
As shown in fig. 6, slots are respectively disposed at both sides of the measuring cylinder fixing plate 14, and the base of the measuring cylinder 12 is inserted into the slots and is in interference fit with the slots.
As shown in fig. 6, a disk 13 is disposed on the vibration table, the disk 13 is fixedly connected to an output shaft of the vibration table, a second rotating electrical machine 24 is disposed on the disk 13, the second rotating electrical machine 24 is an outer rotor electrical machine, an outer rotor of the second rotating electrical machine 24 is fixedly connected to the disk 13, and an inner stator is hollow so as to avoid interference with the output shaft of the vibration table. Two sets of measuring cylinders 12 and measuring cylinder fixing plates 14 are arranged on the disc 13, each measuring cylinder fixing plate 14 is connected with a respective discharging motor, wherein: the measuring cylinder 12 aligned to the second hopper is opened upwards and is positioned at the detection station, the other measuring cylinder 12 is opened downwards and is positioned at the discharge station under the action of the discharge motor, and a second waste sample collecting box is arranged below the discharge station. That is, while one cylinder 12 is in the testing station and receiving a second hopper of sample incoming, the other cylinder 12 is in the discharge station ready to discharge the sample in the cylinder 12.
After all the samples of the second hopper fall into the measuring cylinder 12 of the detection station, the vibrating table is started, the disc 13 drives the two measuring cylinders to vibrate together, and the measuring cylinder 12 of the detection station vibrates to compact the sample particles in the measuring cylinders; at the same time, the measuring cylinder 12 at the discharge station vibrates, so that the sample particles in the measuring cylinder are loosened and fall into the second waste sample collecting box, and the discharge is completed. The processing mode can be used for measuring the tap density of the material for the second time, dumping the material for the previous time, ensuring the cleanness of the measuring cylinder during the next measurement and accelerating the detection efficiency of the vibration density. After the discharging is finished, the discharging motor 16 rotates, and the opening of the measuring cylinder 12 is vertically upward to recover the reset state. Then the second rotating motor acts once to make the measuring cylinder 12 with the upward opening turn to a detection station to prepare for the next detection; at the same time, the graduated cylinder 12 with the tapped sample particles arrives at the discharge station, which is turned upside down, opening downwards, ready for discharge, by the discharge motor 16.
The discharge motor is a stepping motor or a servo motor, and outputs a rotation angle of 180 degrees every time the discharge motor is actuated, so that the measuring cylinder 12 is turned from the opening upward to the opening downward (or from the opening downward to the opening upward).
An output shaft of the vibrating table 19 is fixed at the center of the circle of the disc 13, and the unloading station and the detection station are in central symmetry with the center of the circle of the disc 13. The second rotating motor 24 is a stepping motor or a servo motor, and outputs a rotation angle of 180 ° every time the second rotating motor operates.
An output shaft of the discharging motor 16 is fixed on the center line of the measuring cylinder fixing plate 14, and an open slot aligned with the measuring cylinder 12 is arranged on the disc 13. When the measuring cylinder 12 reaches the unloading station, the unloading motor is turned over by 180 degrees, the measuring cylinder 12 is turned downwards to enter the open slot, and the second waste sample collecting box is positioned below the open slot.
As shown in fig. 6 and 7, the output shaft of the vibration table 19 penetrates through the disc 13 and the second rotating electric machine 24, and a buckle 25 is arranged at the top end of the output shaft, and the buckle 25 tightly presses the second rotating electric machine and the disc 13 against the vibration table 19. The output shaft of the vibrating table vibrates up and down, the outer rotor of the second rotating motor is connected with the disc 13, the inner stator of the second rotating motor is hollow for the output shaft of the vibrating table to pass through, the output shaft and the inner stator are in interference fit, and the buckle 25 mounted on the output shaft limits the axial movement of the second rotating motor.
After the pelletization process is finished, the detection box is opened, and the waste materials in the waste collection device are cleaned at one time.
The operation steps of the invention are as follows:
(1) and (4) preparing, namely performing fluidized bed preparation, wherein the fluidized bed preparation comprises adding base powder, connecting a liquid spraying device, setting the operating parameters of the fluidized bed and operating the fluidized bed. Resetting and checking the detection device so that the detection device is in an initial state and starting the detection device. When the detection device is in an initial state, the sampling mechanism is positioned at a dispersing station, the circular tray 18 is positioned at a horizontal position, and the pressure sensor returns to zero.
(2) The sampling mechanism comprises a sampling mechanism body, wherein a pushing part of the sampling mechanism body extends forwards to serve as the front part of the sampling mechanism body, an inner sleeve of the sampling mechanism body moves towards the direction close to the fluidized bed, an inner sleeve of the sampling mechanism body rotates to enter the fluidized bed under the action of a guide rail, the inner sleeve of the sampling mechanism body is changed from an initial state to an upward opening from the downward opening, and particles in the fluidized bed body enter the inner sleeve of the sampling mechanism body to finish the collection of the samples.
(3) The first visual detection unit completes the detection of the particle size distribution and the angle of repose of the sample particles: the first camera simultaneously obtains images of particles falling in the air and three directions of particle accumulation, the visual system obtains direct images of the falling particles and indirect images of the falling particles in the two plane mirrors 6 from the images, denoising, graying and binaryzation preprocessing are carried out on the photos, and the calculation of particle size distribution of the particles is completed according to the pixel area of each particle image area.
The vision system obtains the direct image of the conical deposit on the circular tray 18 and the indirect image in the two plane mirrors 6 from the image, carries out denoising, graying and binarization preprocessing on the photos of the deposit at three angles, obtains the height data of the conical deposit, calculates the average value of the heights of the conical deposit in the images at three directions as the height H for calculation, and defines the formula according to the angle of repose
The particle angle of repose was calculated. When the measured particle rest angle is not changed, the accumulation is stable, the collector electric telescopic rod retracts, the thick end of the collector valve rod is contacted with the open end of the collector sleeve, the inside of the fluidized bed reactor is isolated from the environment of the detection box, and the particles stop falling. The angle of repose at this time is taken as the calculated angle of repose result.
(4) Sample particle transfer: the pressure sensor 23 measures the mass m on the circular tray 18 at this time0Then, the first rotating motor 9 rotates the circular tray 18 clockwise by 90 degrees, and the particles on the circular tray 18 fall into the measuring cylinder 12 right below through the second hopper 17. While the first rotary motor 9 is oscillated to a small extent in such a manner that the sample on the circular tray 18 can fall down into the measuring cylinder 12. Then, the first rotating motor 9 drives the circular tray 18 to rotate 90 degrees counterclockwise, and the circular tray 18 is reset to prepare for the next detection of the particle size and the angle of repose.
(5) The second visual detection unit is used for detecting the loose packing density and the tap density of the sample particles: after the measuring cylinder 12 below the funnel collects the particles supplied by the circular tray 18, the second camera collects the image of the particles in the measuring cylinder 12, and the vision system gives the particle volume V according to the position information of the sample surface and the scale1According toρ b =m0/V1Calculating the apparent density of the particlesρ b . After the loose density measurement of the particles is completed, the vibration table 19 starts to vibrate. The second camera collects images of the measuring cylinder 12 at fixed intervals in the vibration process until the difference value of the sample volumes is less than 2mL, and the vision system reads the particle volume V2According toρt=m0/V2Calculating the tap density of the particlesρ t According to the formulaε=1-ρ b /ρtAnd HF =ρt/ρ b The particle porosity and hausner ratio were calculated separately.
(6) Unloading a sample: the disc 13 is driven by the second rotating motor to rotate 180 degrees, the measuring cylinder 12 filled with sample particles is transferred to the unloading station from the detection station below the second hopper, and meanwhile, the empty measuring cylinder 12 is transferred to the detection station, the opening of the empty measuring cylinder 12 faces upwards, and the second hopper is ready to receive sample incoming materials. Then the discharge motor 16 of the discharge station drives the measuring cylinder 12 to rotate downwards by 180 degrees until the opening of the measuring cylinder 12 is downward, and the measuring cylinder is positioned right above the second waste sample collecting box 20 to wait for the opening of the vibrating table. The vibration table 19 vibrates so that the particles after tap density measurement can fall to the second waste collection box 20. When unloading, the shaking table does not vibrate for unloading, but when the tap density of the next time is measured and vibrated, the measuring cylinder 12 of the detection station and the measuring cylinder 12 of the unloading station vibrate simultaneously, and the processing mode can be used for measuring the tap density of the material for the second time and dumping the material for the last time, so that the cleanness of the measuring cylinder during the next time is ensured, and the vibration density detection efficiency is accelerated. After the vibration is finished, the discharging motor 9 rotates, the opening of the measuring cylinder 12 is vertically upwards recovered to a reset state, and the measuring cylinder waits to be transferred to a detection station to prepare for next detection.
The embodiments described in this specification are merely illustrative of implementations of the inventive concept and the scope of the present invention should not be considered limited to the specific forms set forth in the embodiments but rather by the equivalents thereof as may occur to those skilled in the art upon consideration of the present inventive concept.
Claims (9)
1. The detection device is arranged outside a reaction chamber of the fluidized bed, and is provided with a sealed shell, a sample acquisition mechanism capable of taking out a sample from the reaction chamber, and a first visual detection unit which is positioned in the shell and shoots the falling process of the taken sample in the shell;
the method is characterized in that: a second visual detection unit for detecting the apparent density and the tap density of the sample is arranged in the shell, the sample is transferred from the first visual detection unit to the second visual detection unit by the sample transfer mechanism, and image information obtained by the first visual detection unit and the second visual detection unit is input into the image processing system;
the circular tray receives a sample falling from the sample acquisition mechanism, the first camera shoots the falling process of the sample and an image of a sample deposit on the circular tray, and the image processing system obtains particle size information from the falling image of the sample and obtains an angle of repose α from the image of the sample deposit;
the sample transfer mechanism comprises a rotating motor and a collecting funnel, the rotating motor is fixedly connected with a supporting shaft of the circular tray, the supporting shaft is fixed at the lower end of the circular tray and is positioned on a circular central axis of the circular tray, the circular tray is upright to receive a falling sample when the rotating motor is at a first position, and the circular tray is inclined in a vibrating mode to pour all the samples on the circular tray into the collecting funnel when the rotating motor is at a second position;
the second visual detection unit comprises a measuring cylinder for receiving the materials from the collecting funnel, a measuring cylinder fixing plate, a light source, a vibration table and a second camera, the measuring cylinder is fixed on the measuring cylinder fixing plate, the measuring cylinder fixing plate is arranged on the vibration table, and the second camera and the light source shoot a sample image in the measuring cylinder; the image processing system obtains the apparent density rho of the particles from the sample image in the measuring cylinder before the vibration table is startedbJudging a vibration end point by a sample image in the measuring cylinder in the vibration process of the vibration table and obtaining the tap density rho of the particlest；
The first visual detection unit comprises a plurality of plane mirrors and a plurality of surface light sources, the plane mirrors and the surface light sources are distributed at intervals, the plane mirrors and the surface light sources are enclosed to form a regular polygon area with a notch, the first camera is arranged at the notch, and the circular tray is located in the regular polygon area.
2. The apparatus for the on-line detection of properties of granules in a fluid bed granulation process as defined in claim 1, wherein: the circular tray is positioned in the center of the regular polygon area, and a sample blanking port of the sample acquisition mechanism is aligned with the circle center of the circular tray; the sample deposit image comprises a direct image of the deposit on the circular tray and indirect images of the deposit on the circular tray in each plane mirror; the image processing system acquires height data of the deposit in each image, and takes the average height as the height for calculationH, calculating the angle of repose
R is the radius of the circular tray.
3. The apparatus for the on-line detection of properties of granules in a fluid bed granulation process as claimed in claim 2, wherein: the first camera shoots an image of a deposit on the circular tray in real time, and the sample collection mechanism stops sampling when the conical angle of the image of the deposit is not changed; after the sample collection mechanism stops sampling, the pressure sensor obtains the mass m of the sample particles on the circular tray0(ii) a Mass m0After the taking, the circular tray is inclined in a vibration mode to pour all the samples on the circular tray into a collection funnel, so that the samples enter the measuring cylinder; apparent density ρb＝m0/V1，V1A scale for locating the sample particles before vibration, shot by the second camera, in the measuring cylinder; tap density ρt＝m0/V2，V2The vibrated sample particles photographed by the second camera are located on a scale in the graduated cylinder.
4. The apparatus for the on-line detection of properties of granules in a fluid bed granulation process as claimed in claim 3, wherein: in the first visual detection unit, the adjacent surface light sources and the plane mirrors form an included angle of 120 degrees, the number of the surface light sources is 3, and the number of the plane mirrors is 2; the surface light source and the plane mirror are enclosed into a regular hexagon area with a gap.
5. The apparatus for the on-line detection of properties of granules in a fluid bed granulation process as defined in any of claims 1 to 4, wherein: the collecting funnel consists of a first funnel and a second funnel, the second funnel receives the transfer blanking of the circular tray, and the first funnel receives the overflow blanking when the circular tray is in an upright state; the second funnel is communicated with the first funnel, the outlet of the second funnel is aligned in the measuring cylinder, and the outlet of the first funnel is aligned with the first waste sample collecting box.
6. The apparatus for the on-line detection of properties of granules in a fluid bed granulation process as claimed in claim 5, wherein: the measuring cylinder fixing plate is connected with a discharging motor, and the discharging motor is fixed on the table top of the vibration table; when the opening of the measuring cylinder is vertically upward, the discharging motor is positioned at a visual detection position; when the opening of the measuring cylinder is vertically downward, the discharging motor reaches the discharging position; in the discharge position, the sample in the measuring cylinder falls into the second waste sample collecting box.
7. The apparatus for the on-line detection of properties of granules in a fluid bed granulation process as claimed in claim 6, wherein: when the measuring cylinder is positioned at the detection station, the opening of the measuring cylinder is upward, so that a sample supplied by the circular tray through the funnel can be collected, and at the moment, the opening of the measuring cylinder positioned at the unloading station is downward; after the apparent density is obtained by the image processing system, the vibration table starts to vibrate; the image processing system can obtain tap density through the volume of the sample in the graduated cylinder in the detection station, and the station of unloading can be retrieved the sample that is surveyed in waste collection box through the vibration.
8. The apparatus for the on-line detection of properties of granules in a fluid bed granulation process as claimed in claim 7, wherein: a disc is arranged on the vibrating table, a second rotating motor is arranged on the disc, the second rotating motor is an outer rotor motor, an outer rotor of the second rotating motor is fixedly connected with the disc, and the inner stator is hollow; an output shaft of the vibrating table penetrates through the disc and the second rotating motor, a buckle is arranged at the top end of the output shaft, and the second rotating motor and the disc are tightly abutted to the vibrating table through the buckle; and two measuring cylinders and measuring cylinder fixing plates are arranged on the disc, each measuring cylinder fixing plate is connected with a respective unloading motor, an opening of the measuring cylinder aligned with the second hopper is upward and positioned at a detection station, the other measuring cylinder is positioned at an unloading station, and the second waste sample collecting box is positioned below the unloading station.
9. The apparatus for the on-line detection of properties of granules in a fluid bed granulation process as claimed in claim 8, wherein: the sample collecting mechanism is positioned outside the shell and mainly comprises a collecting sleeve, a piston rod, a collecting piston at the end of the piston rod and a sampling pushing member, wherein the sampling piston is in sealing fit with the sampling sleeve; when the sample collection mechanism stops sampling, the sampling piston isolates the inlet and the outlet of the sampling sleeve; a speed reducing guide pipe is arranged between the sampling sleeve and the shell, the speed reducing guide pipe is an elbow pipe, an inlet of the speed reducing guide pipe is communicated with an outlet of the sampling sleeve, an outlet of the speed reducing guide pipe is communicated with an inner cavity of the shell, an outlet of the speed reducing guide pipe is used as a sample blanking port of the sample collecting mechanism, and an inlet of the speed reducing guide pipe is higher than an outlet of the speed reducing guide pipe.
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