JP4472494B2 - Powder processing equipment - Google Patents

Description

  The present invention relates to a granular material processing apparatus that performs granulation, coating, and drying of granular material.

  Granule processing equipment that performs granulation, coating and drying of granular materials includes fluidized bed equipment, agitation granulators, centrifugal tumbling granulators, etc. Widely used in the field.

  In general, a fluidized bed apparatus performs granulation, coating, and drying while forming a fluidized bed by floating and flowing a granular material in a processing container with a fluidized gas introduced from the bottom of the processing container. Among this type of fluidized bed apparatus, those that involve rolling, jetting, stirring, etc. of granular particles are called composite fluidized bed apparatuses, and typically rotate to the bottom of a fluidized bed container. There are a rolling fluidized bed apparatus having a body and a so-called Wurster fluidized bed apparatus in which a draft tube (inner tower) is installed inside a fluidized bed container.

  The agitation granulator is an apparatus that disperses and kneads a solid-liquid by agitation with an agitation blade and granulates (for example, see Patent Document 1 below).

  A centrifugal rolling granulator is an apparatus that rolls and mixes granular materials on a rotating disk and sprays a binder liquid thereon to perform granulation (see, for example, Patent Document 2 below).

  In operations that perform granulation, coating, etc. using the above-described powder processing apparatus, based on past operation data, operator experience, etc., air supply conditions, exhaust conditions, binder substances and film agent substances The operational factors such as the addition conditions (if sprayed in liquid form, spray amount, spray liquid speed, etc.) are often set and fine-tuned according to the situation, climate change, raw material quality variation Depending on factors such as operator skill and shifts, products with the desired quality may not be obtained with sufficient reproducibility. For this reason, from the viewpoint of process validation, various techniques for measuring physical property values such as the particle size of the granular particles during the treatment process and using the measured values for controlling the operation factor and determining the granulation end point have been proposed. .

  For example, in the following Patent Document 3, a granular material is introduced by injecting a high-pressure gas from the inside of the granulation container into the granular material extraction tube protruding from the inside of the granulation container, and this is captured by an adhesive film. At the same time, the captured granular material is imaged, and the particle size and sphericity of the granular particle are obtained based on the obtained video information.

  In Patent Document 4 below, powder particles are sampled from the inside of a fluidized bed container by a screw conveyor type sampling device, the sampled powder particles are guided to a conduit, and the particles freely fall in the conduit by gravity. The particle diameter is measured with a laser particle diameter sensor.

  In the following Patent Document 5, the granulated particles taken out from the inside of the fluidized bed container are converted into temporary particles by a high-speed air flow to eliminate the overlapping of the particles, and by observing this from multiple directions by a light transmission method, The three-dimensional morphology and particle distribution of the particle are measured.

  In the following Patent Document 6, the powder particles are sucked from the inside of the fluidized bed container and guided to the measurement cell, the particles are irradiated with light in the measurement cell, and the diffraction / scattered light from the particles is received, The particle size distribution of the particles is measured.

In the following Patent Document 7, infrared light is irradiated from the moisture detection adapter arranged facing the inside of the fluidized bed container toward the powder flowing in the fluidized bed container, and light reflected by the powder particles is received. The moisture content of the granular particles is measured based on the attenuation amount (absorption amount) of infrared rays.
JP-A-5-236 Japanese Patent Laid-Open No. 6-262054 WO97 / 15816 publication JP 7-333113 A Japanese Patent No. 3450405 JP-A-11-216351 JP-A-6-55054

  In the technique described in Patent Document 3, it is difficult to manage the number of particles captured by the adhesive film, and sometimes a large amount of granular particles adhere to the adhesive film and cannot be measured. Moreover, since the particles captured by the adhesive film are not handled as a product and discarded, the product is lost.

  In the techniques described in Patent Documents 4 to 6, powder particles sampled from the inside of a processing vessel are guided to a measurement site, and particles passing through the measurement site (in a moving state) are detected by optical means. For this reason, the time during which particles can be detected is short, and the reliability of measurement data may not be sufficiently obtained, and the physical property values that can be measured are limited to the particle diameter and particle form.

  Since the technique described in Patent Document 7 detects powder particles (moving) in a fluidized bed container with a moisture detection adapter, the detection amount depends on the distance of the particles from the moisture detection adapter. In some cases, the measurement data may not be sufficiently reliable.

  The subject of this invention is enabling it to measure the physical property value of a granular material particle | grain with high precision during processing operation of a granular material.

  An object of the present invention is to make it possible to accurately measure various physical properties of powder particles.

In order to solve the above problems, the present invention moves in a processing container in a powder processing apparatus that performs at least one of granulation, coating, and drying while moving the powder in the processing container. A particle capturing unit having a predetermined volume that captures and accommodates a part of the granular material, a probe having a translucent part provided at least at a part around the particle capturing unit, and a particle capturing unit of the probe. A measurement unit that measures the physical property value of the granular particles by irradiating the granular material with light through a translucent part, and the probe is provided through an introduction part provided on the wall of the processing container. In addition, the particle capturing unit is movably disposed between a capturing position capable of capturing the granular material inside the processing container and a measuring position where the measurement unit performs measurement outside the processing container, and purges the particle capturing unit. providing a structure that includes a gas passage for supplying air

  Here, the physical property values of the powder particles include particle diameter, particle shape, particle size distribution, component content (component concentration), elution control performance, moisture content, and the like.

  In addition, the measurement unit used in the present invention includes a measurement device that measures the physical property value of the granular material by near infrared spectroscopy, Raman spectroscopy, or infrared spectroscopy. For example, near-infrared spectroscopy irradiates a measurement object with light in the near-infrared region (wavelength range 800-2500 nm), detects the reflected light or transmitted light, and analyzes the physical property value of the object. This is a method for obtaining. According to this near-infrared spectroscopy, in addition to morphological properties such as the particle diameter of powder particles, it is possible to determine compositional properties such as component content and moisture content. Furthermore, chemical properties such as particle elution control performance can be evaluated based on these properties. For example, in the coating operation of drug particles, the performance of the elution control film can be determined from the content of the film agent substance on the particle surface determined by near infrared spectroscopy, and the elution characteristics of the drug particles can be evaluated.

  Further, the translucent part provided at least at the periphery of the particle trapping part has a configuration in which at least a part of the wall surface constituting the particle trapping part is formed of a translucent material such as transparent glass, A configuration in which at least a part is opened to the outside is included. In the latter case, the entrance / exit of the powder body with respect to the particle trapping part may be a translucent part.

In the present invention, the probe includes a particle trapping unit having a predetermined volume, and a part of the powder moving in the processing container can be captured and sampled by a predetermined amount by the particle trapping unit of the probe. Then, after capturing the granular material by the particle capturing portion of the probe, the probe is moved to a measurement position outside the processing container, and at the measurement position, the light transmitting portion is transferred to the granular material accommodated in the particle capturing portion of the probe. The physical properties of the powder particles are measured by irradiating with light. At this time, since a predetermined amount of the granular material is accommodated in the particle capturing portion of the probe, the accumulated thickness (or accumulated width) of the granular material is constant with respect to reflection or transmission of the irradiated light. Moreover, since the granular particles in the particle trapping part are in a stationary state at the time of measurement, it is possible to sufficiently secure the detection time necessary for measuring the physical property values. For this reason, it is possible to measure the physical property value of the granular particles with high accuracy. After the measurement of the granular particles, the probe (particle capturing unit) is moved to the capturing position inside the processing container (the probe may be rotated after the movement), and purge air is supplied from the gas passage. Then, the granular material accommodated in the particle | grain capture | acquisition part can be blown off with purge air, and can be returned in a processing container. Moreover, when not capturing a granular material, by supplying purge air, it is possible to prevent the granular material moving in the processing container from entering the particle capturing portion.

  In the above configuration, a gas passage that supplies purge air to a gap between the introduction portion of the processing container and the probe may be provided in at least one of the introduction portion and the probe. Due to the purge air supplied through the gas passage, the granular material in the processing container leaks to the outside through the gap, or foreign matter enters the processing container from the outside through the gap. Evil effects such as doing are avoided (air seal).

  Hereinafter, embodiments in which the present invention is applied to a fluidized bed apparatus will be described with reference to the drawings.

  FIG.1 and FIG.2 has shown typically the example of 1 structure of the fluidized bed apparatus concerning this embodiment.

  A filter system 2 is installed in the upper space of the fluidized bed container (processing container) 1, and a gas dispersion plate 3 composed of a perforated plate (or metal mesh) such as punching metal is disposed at the bottom of the fluidized bed container 1. . A fluidizing gas A such as hot air supplied from an air supply duct (not shown) to the air supply chamber 5 is introduced into the fluidized bed container 1 through the gas dispersion plate 3. A spray nozzle 4 for spraying a spray liquid (film agent liquid, binder liquid, etc.) is installed inside the fluidized bed container 1.

  The granular material M accommodated in the fluidized bed container 1 is suspended and fluidized by the fluidized gas A introduced into the fluidized bed container 1, whereby the fluidized bed of the granular material M in the fluidized bed container 1. Is formed. Then, spray liquid (film agent liquid, binder liquid, etc.) is sprayed from the spray nozzle 4 toward the fluidized bed of the granular material M. At the same time that the granular material particles M are wetted by the spray liquid sprayed from the spray nozzle 4, for example, a mist of the film agent liquid, the solid component contained in the film agent liquid adheres to the surface of the granular particle M, After drying and solidifying, a coating layer is formed on the surface of the powder particles M (coating). Alternatively, the powder particles M are wet, adhered and agglomerated by a spray liquid sprayed from the spray nozzle 4, for example, a mist of a binder liquid, and dried to grow into particles having a predetermined diameter (granulation).

  In this embodiment, the probe 6 is attached to the wall portion of the fluidized bed container 1, particularly the peripheral wall portion 1 a of the flow chamber that becomes the flow space of the granular material M, and the measurement unit 7 is disposed on the side thereof.

  The probe 6 has, for example, a circular particle shape such as a circular shape or a quadrangular shape, and a concave particle capturing portion 6a having a predetermined volume in a part thereof. In this embodiment, in the same figure of the particle capturing part 6a, the upper part is an opening 6a1, and the lower part is a light transmitting part 6a2 made of a light transmitting material such as transparent glass. Further, the wall surface on the inner side of the particle trapping portion 6a (the inner side of the fluidized bed container 1) is an inclined surface 6a3 having a predetermined inclination angle. Further, a gas passage 6a4 (see FIG. 3) for supplying the purge air P2 is opened on the wall surface on the outer side of the particle trapping portion 6a (the outer side of the fluidized bed container 1). The purge air P2 is used when the granular material M accommodated in the particle capturing part 6a is returned into the fluidized bed container 1 {see FIG. 3 (c)} or when the granular material is not captured {FIG. 3 (d). Reference} is supplied to the particle trap 6a through the gas passage 6a4.

  The probe 6 is slidably inserted into a cylindrical introduction portion 1a1 that protrudes from the peripheral wall portion 1a of the fluidized bed container 1 (such as a cylindrical shape or a rectangular tube shape corresponding to the cross-sectional shape of the probe 6). . In addition, a gas passage 1a11 (see FIG. 3) for supplying purge air P1 to a gap between the probe 6 and the introduction part 1a1 (a guide gap for guiding the sliding movement of the probe 6) is provided in the introduction part 1a1. ing. The gap is sealed {see FIG. 3} by purge air P1 supplied to the gap via the gas passage 1a11.

  In this embodiment, the measuring unit 7 includes a height-adjustable measuring table 7a, slide driving means mounted on the measuring table 7a, for example, an air cylinder 7b, and an optical sensor installed at a predetermined position of the measuring table 7a. For example, a near-infrared sensor 7c is provided. The rod 7b1 of the air cylinder 7b is connected to the outer end of the probe 6, and the probe 6 is slid along the introduction portion 1a1 by the operation of the air cylinder 7b. The near-infrared sensor 7c is a reflection type in this example, and a light projecting unit that irradiates near-infrared light and a light-receiving unit that receives reflected light of the irradiated light are accommodated in the same casing. . The installation position of the near infrared sensor 7c is such that when the probe 6 is slid to the rear side by the operation of the air cylinder 7b and reaches a predetermined position, the light projecting part and the light receiving part are the light transmitting part 6a2 of the particle capturing part 6a. And a predetermined distance (measurement distance). Measurement data (received light of reflected light) by the near-infrared sensor 7c is transmitted to an arithmetic processing device (not shown) via a transmission means such as an optical fiber, and the spectral processing of the reflected light is performed by the arithmetic processing device. Is called. And physical property values, such as the content (component density | concentration) of the granular material particle | grains M, are calculated | required based on the spectrum analysis.

  The probe 6 has at least a particle trapping portion 6a inside the fluidized bed container 1, and a trapping position where the particle trapping part 6a can trap the powder M flowing in the fluidized bed container 1 {FIG. 1, FIG. ), (C), position shown in (d)}, and the light transmitting part 6a2 of the particle capturing part 6a faces the light projecting part and the light receiving part of the near infrared sensor 7c disposed outside the fluidized bed container 1. The probe 6 is slidable between two measurement positions (positions shown in FIGS. 2 and 3B), and the probe 6 is positioned and slid by an air cylinder 7b.

  FIG. 3A shows a state at the time of capturing the powder M. The probe 6 is in the capture position, and the gap between the probe 6 and the introduction portion 1a1 is sealed with the purge air P1. The position of the particle trapping portion 6a of the probe 6 is set near the inner surface of the peripheral wall portion 1a of the fluidized bed container 1, for example. Part of the granular material M flowing in the fluidized bed container 1 enters the particle trapping portion 6a of the probe 6 when flowing downward, and accumulates in the particle trapping portion 6a. In this way, a part of the granular material M flowing in the fluidized bed container 1 is captured by the particle capturing unit 6a of the probe 6, and when the granular material M exceeding the volume of the particle capturing unit 6a is deposited, the air is collected. The cylinder 7b is operated to slide the probe 6 from the capture position to the measurement position. In addition, by forming at least one of the introduction portion 1a1 and the probe 6 with a self-lubricating material, for example, a resin material such as PTFE (Teflon: registered trademark), the powder particles are encased in the gap portion. It is also possible to prevent the operation failure caused by it.

  FIG. 3B shows a state in which the probe 6 is slid to the measurement position. Part of the granular material M deposited at the capturing position over the volume of the particle capturing part 6a (the part rising from the opening 6a1 of the particle capturing part 6a) is measured at the position where the probe 6 passes through the inside of the introducing part 1a1. When the slide portion moves to the fluidized bed container 1 by the introduction portion 1a1 and is returned to the fluidized bed container 1 (in the drawing, the size of the gap between the probe 6 and the introduction portion 1a1 is larger than the actual size). Shown quite exaggerated). Therefore, when the probe 6 slides to the measurement position, a predetermined amount (a constant amount) of the granular material M corresponding to the volume of the particle capturing unit 6a is accommodated in the particle capturing unit 6a. Thus, after capturing a predetermined amount (a constant amount) of the granular material M by the particle capturing part 6a of the probe 6, the physical property value of the granular material particle M is measured at the measurement position. That is, the near infrared light is irradiated from the light projecting portion of the near infrared sensor 7c to the granular layer M through the light transmitting portion 6a2 of the particle capturing portion 6a, and the reflected light reflected by the granular particles M is near. Light is received by the light receiving portion of the infrared sensor 7c. The light reception data of the reflected light is transmitted to an arithmetic processing device (not shown) via a transmission means such as an optical fiber, and spectrum analysis or the like is performed by the arithmetic processing device. And physical property values, such as the content (component density | concentration) of the granular material particle | grains M, are calculated | required based on the spectrum analysis. Thus, since the physical property value is measured in a state where the probe 6 is positioned at the measurement position and a certain amount of the powder M accommodated in the particle trapping portion 6a is stationary, the proximity to the powder layer M is measured. The measurement distance of the infrared sensor 7c and the layer thickness of the granular material layer M are constant, thereby improving the reliability of the measurement data and measuring the physical property value of the granular particle M with high accuracy. The near infrared sensor may be a transmission type. In this case, the light projecting unit and the light receiving unit of the near-infrared sensor are arranged to face each other through the powder layer M in the particle capturing unit 6a. Further, while the probe 6 is slid from the capture position to the measurement position, it is preferable to stop the supply of the purge air P1 so that the powder M accommodated in the particle capture unit 6a is not scattered by the purge air P1.

  After the measurement of the physical property values of the powder particles M is completed, the probe 6 is slid again to the capture position as shown in FIG. Then, purge air P2 is supplied to the particle trapping portion 6a via the gas passage 6a4, and the granular material M in the particle trapping portion 6a is discharged by the purge air P2 and returned to the fluidized bed container 1. During the sliding movement of the probe 6 from the measurement position to the capture position, it is preferable to stop the supply of the purge air P1 so that the granular material M accommodated in the particle capture unit 6a is not scattered by the purge air P1.

  As shown in FIG. 3D, it is preferable that the purge air P2 is continuously supplied to the particle trapping unit 6a even after the powder M is discharged from the particle trapping unit 6a. Thus, even when the particulate matter M is not captured (when measurement is not performed), the probe 6 is moved while preventing the particulate matter M flowing in the fluidized bed container 1 from entering the particle capturing portion 6a. It can be in the state where it is located at the capture position. When capturing the powder M (when performing measurement), the supply of the purge air P2 can be stopped to quickly shift to the capturing operation. The pressure of the purge air P2 is preferably relatively low so as not to hinder the smooth flow of the granular material M in the fluidized bed container 1.

  In the above embodiment, the purge air P2 is used as means for returning the granular material M in the particle trapping portion 6a of the probe 6 into the fluidized bed container 1 {FIG. 3 (c)}, but the probe 6 is 180 degrees. Rotate (a separate rotation driving means for the probe 6 is provided) so that the opening 6a1 of the particle trapping portion 6a faces downward and the granular material M in the particle trapping portion 6a is returned to the fluidized bed container 1. Also good. In this case, purge air P2 may be used in combination, or supply of purge air P2 may be stopped. In addition, the present invention is not limited to the fluidized bed apparatus as described above, and powders such as composite fluidized bed apparatuses such as Wurster type fluidized bed apparatus and rolling fluidized bed apparatus, stirring granulators, centrifugal rolling granulators and the like. The present invention can be similarly applied to a particle processing apparatus.

It is sectional drawing which shows typically the example of 1 structure of the fluidized-bed apparatus which concerns on embodiment (a state in which a probe exists in a capture position). It is sectional drawing which shows typically the example of 1 structure of the fluidized-bed apparatus which concerns on embodiment (a state in which a probe exists in a measurement position). It is sectional drawing which shows the peripheral part of a probe typically.

Explanation of symbols

1 Fluidized bed container (processing container)
1a Peripheral wall portion 1a1 Introduction portion 1a11 Gas passage 6 Probe 6a Particle trapping portion 6a2 Translucent portion 6a4 Gas passage 7c Near infrared sensor P1 Purge air P2 Purge air

Claims (3)

In the granular material processing apparatus that performs at least one of granulation, coating, and drying while moving the granular material in the processing container,
A probe having a particle capturing part having a predetermined volume for capturing and accommodating a part of the powder particles moving in the processing container, and a light transmitting part provided in at least a part of the periphery of the particle capturing part; A measurement unit that measures the physical property value of the granular particles by irradiating the granular material accommodated in the particle capturing unit of the probe with light through the translucent unit;
The probe is measured by the measurement unit outside the processing container and a capturing position where the powder can be captured inside the processing container via an introduction part provided on the wall of the processing container. A powder processing apparatus comprising a gas passage that is movably disposed between a measurement position to be measured and that supplies purge air to the particle capturing unit .   The gas passage for supplying purge air to a gap between the introduction portion of the processing container and the probe is provided in at least one of the introduction portion and the probe. Powder processing equipment. The said measurement part irradiates the near-infrared light to the said granular material, and measures the physical-property value of this granular material particle | grain by analyzing the transmitted or reflected light, It is characterized by the above-mentioned. Or the granular material processing apparatus of 2.

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