JPH0232932B2 - RYUSHIKAKOHOHOOYOBISOCHI - Google Patents

Description

[Detailed description of the invention]

Industrial Application Field This patent relates to a particle processing method and apparatus used for powder mixing, granulation, coating, etc. Conventional technology For example, when adding liquid to powder and granulating it, stirring with stirring blades disperses, mixes, and
Stirring granulation method in which particles are formed by kneading; Fluid granulation method in which liquid is sprayed onto a layer of powder dispersed and mixed in an air stream to cause the powders to adhere and aggregate to form particles;
The rolling granulation method involves mixing powders by rolling them in a rotating container, spraying a liquid on top of the mixture, and making the powders adhere to each other and coagulate. Extrusion granulation method to form particles, and spraying to form particles by atomizing a solution in which the ingredients to be formed into particles are dissolved or suspended using a nozzle or rotating disk, and then drying it with hot air or dry air. Granulation method is used. Problems to be Solved by the Invention When processing particles to produce products with high added value, particles with uniform particle size, good sphericity, and high bulk density are often required. As a means for forming particles with uniform particle size, sphericity, and high bulk density, each of the above granulation methods has its own drawbacks. That is, particles made by the known stirring granulation method have a wide particle size distribution, particles made by the fluidized granulation method have a small bulk density, and particles made by the rolling granulation method have a wide particle size distribution. Furthermore, particles produced by extrusion granulation have a narrow particle size distribution but low sphericity. Furthermore, particles produced by the spray granulation method have good sphericity but a wide particle size distribution. On the other hand, Utility Model Publication No. 53-11419 describes a crushing and granulating device equipped with a rotating blade and a fixed blade.
Particles formed by crushing and granulation have a wide particle size distribution, and it is difficult to maintain sphericity at a practically satisfactory level. As described above, from the viewpoints of particle size distribution, sphericity, and bulk density, there is currently no practically satisfactory granulation method. The main object of the present invention is to provide a solution to the above-mentioned problems found in conventional granulation methods. Means for Solving the Problems In view of the above object, the present invention is designed to charge powder and a predetermined amount of liquid into a container, and collide the particles flowing in the stirring direction during the granulation process with a fixed blade or a rotating blade. At the same time, the particles are sandwiched between the stirring blade and the fixed blade or the rotating blade, and coarse particles are selectively crushed by the interaction between the stirring blade and the fixed blade or the rotating blade. , a particle processing method in which adhesion agglomeration, rolling compaction, and crushing grading are performed in parallel while grading action is performed, and powder and a predetermined amount of liquid are placed in a container and rotated at high speed. In a particle processing device that uses stirring blades to agitate powders to adhere and bond them to form particles, a rotating shaft supported at the center of a cylindrical container has an inclined surface that slopes downward in the direction of rotation. A particle processing device is equipped with a stirring blade having a horizontal surface, the stirring blade is placed close to the bottom of a cylindrical container, and a fixed blade or a rotary blade is installed close to the horizontal surface of the stirring blade. This is the summary. Function: A stirring blade that rotates at high speed is attached to the bottom of a cylindrical container, and a fixed blade or rotating blade with a sharp end is installed directly above the stirring blade, and the relative movement between the stirring blade and the fixed blade or rotating blade is utilized. This promotes particle size regulation and forms particles with high bulk density and excellent sphericity and uniform particle size distribution. Example 1 The stirring blade 1 is as shown in FIG. 1 AB, FIG. 2, and FIG. 3.
As shown in the figure, there is an inclined surface 1a having a downward slope in the direction of rotation and an inclination angle of 25 to 50 degrees, which functions as a swirling flow generating section, and a slanted surface 1a which is connected to the rear of the inclined surface and functions as a grain regulating section. It is composed of a horizontal portion 1b having a roughly horizontal or nearly horizontal gently curved surface. A fixed blade 2 provided directly above the stirring blade 1 and close to the inner peripheral wall surface of the cylindrical container 4.
Alternatively, the rotary blade 3 has a radial length of 1/3 or less of the radius of the cylindrical container 4 as measured from the inner circumferential wall surface of the cylindrical container 4 toward the center, and has a sharp tip;
The blade should be positioned 1 mm to 5 mm above the horizontal portion 1b of the stirring blade 1, more preferably 1.5 mm to 2.5 mm vertically above the horizontal portion 1b of the stirring blade 1, and the blade surface should be approximately horizontal or slightly horizontal. Install it at a slope. One or more fixed blades 2 are installed in the cylindrical container 4 depending on the capacity of the cylindrical container 4. On the other hand, the rotary blade 3 is attached to a rotary blade (not shown) suspended from the top of the cylindrical container 4 or to a rotary shaft 5a supported with its axis aligned with the rotary shaft 5 of the stirring blade 1. , rotates in the opposite direction to the rotation direction of the stirring blade 1. Like the fixed blade 2, the rotary blade 3 is attached so that its blade surface is substantially parallel to the horizontal portion 1b of the stirring blade 1. The functions of the above-mentioned stirring granulation device will be explained based on an example conducted using a small experimental machine with a diameter of 100 mm. The inclination of the swirling flow generating portion 1a of the stirring blade 1 of this device is
30 degrees, its length is 30 mm, and the length of the grain regulating section 1b is 20 mm.
It is almost horizontal. There is a distance of 0.5 mm between the tip of the stirring blade along the rotational direction and the inner wall surface of the cylindrical container 4.
Maintaining distance. This stirring blade 1 is
Rotates at 1500rpm. At one point on the container wall, the width in the container diameter direction is 15 mm, the circumferential length is 13 mm, and the thickness is 0.2 mm.
The fixed blade 2 is installed with the blade surface oriented in a substantially horizontal direction. The mounting position of the fixed blade 2 was varied in the vertical distance from the blade surface 1b of the particle size regulating part of the stirring blade 1 between 1.0 mm and 30 mm, and the influence of the mounting position was investigated. In the powder treatment, 60 parts by weight of lactose, 10 parts by weight of microcrystalline cellulose, and 30 parts by weight of cornstarch were placed in the cylindrical container 4, and 35 c.c. of water was added dropwise while stirring. Stir at 1500 rpm for about 10 minutes. The obtained particles were dried, and the particle size distribution and bulk density were measured, and the particle shape was observed. The measurement results are shown in FIGS. 4A to 4F and Table 1 below. Incidentally, FIG. 4G shows the particle size distribution of particles obtained in a comparative example described later using a conventional stirring blade without a horizontal particle size regulating part and a fixed blade.

[Table] From the above experimental results, the installation position of the fixed blade 2 is expressed as the vertical distance measured from the particle size regulating part 1b of the blade 1.
When the particle size was less than mm, the particle size distribution became extremely uniform and comparable to the particle size distribution of particles obtained by a known extrusion granulation method. Regarding the sphericity, as shown in Fig. 5, the granules obtained by the present invention have the following properties:
It was confirmed that the level was maintained at a level comparable to that of the rolling granulation method or the spray granulation method. Comparative Example In the above Example 1, the stirring blade 1 having both the inclined surface 1a that sloped downward in the direction of rotation and the substantially horizontal grain regulating section 1b was used, but the effect of the inclined surface and the grain regulating surface was confirmed. Therefore, an experiment was conducted using the same recipe and under the same conditions by combining a conventional stirring blade that does not have a horizontal particle size regulating part 1b with the fixed blade 2 used in the above experiment. The results are shown in FIG. 4G. As can be understood from FIGS. 4A to 4G, conventional stirring blades that do not have the horizontal part 1b that functions as a grain regulating part do not have a grain regulating effect, and are inclined downward in the direction of rotation. It was confirmed that, for the first time, the interaction between the stirring blade 1 of the present invention, which has both a flat surface and a substantially horizontal surface, and the fixed blade 2 exerts a particle size regulating function that is effective in maintaining sphericity. Example 2 Next, instead of the fixed blade 2, as shown in FIG. 2, a rotary blade 3 whose surface facing the stirring blade 1 forms a horizontal plane and whose length in the rotation radius direction is 15 mm is prepared. was attached to a second rotating shaft 5b arranged concentrically with respect to the rotating shaft 1a of the stirring blade 1. In this state, the blade surfaces of the rotary blades 3 are arranged facing each other above the horizontal part 1b of the stirring blade 1 with a vertical separation distance of 2.5 mm, and the blades are rotated so that their outer ends move along the inner surface of the circumferential wall of the container 4. The blade 3 was driven to rotate. In this example, the granulation behavior was observed while changing the rotation speed of the rotary blade 3 over a range of 0 to 500 rpm. In addition, the rotation speed of stirring blade 1 is
At 1000 rpm, the recipe and operating conditions were set the same as in Example 1 above. The measurement results are shown in FIGS. 6A to 6D. As can be seen from this, as the rotational speed of the rotary blade 3 increases, the amount of coarse particles decreases, but on the contrary, the amount of fine particles increases. However, overall the particle size distribution is significantly more uniform than with conventional methods. Hereinafter, the granulation characteristics by the apparatus of the present invention will be explained in detail. As the stirring blade rotates at high speed, the particle layer generates a swirling flow due to the action of the swirling flow generating portion 1a, which imparts a rolling compaction effect to the particles and promotes spheroidization. When the particles move along the swirling flow generating section 1a and reach the horizontal section of the stirring blade 1, that is, the particle regulating section 1b, the particles with large particle sizes are crushed by hitting the sharp tip of the fixed blade 2, and the particle size is reduced. The small particles rotate and move to avoid collision with the fixed blade 2. Further, coarse particles that cannot pass through the gap between the horizontal portion 1b of the stirring blade 1 and the fixed blade 2 are crushed. In this way, spheroidization by the rolling compaction effect of the swirling flow and particle size regulation by crushing or grinding of coarse particles are carried out in parallel. Fixed blade 2 for particle size regulating effect
This occurs due to the interaction between the particle size regulating portion 1b of the stirring blade 1, and in this case, the vertical distance between the horizontal portion 1b of the stirring blade 1 and the fixed blade 2 is important. That is, when the vertical distance is large, the effect of crushing or grinding coarse particles is small, and the average particle size of the obtained particles increases,
On the other hand, when the vertical distance is small, particles with a relatively small particle size are also crushed by the fixed blade 2 while rolling on the particle size regulating part 1b of the stirring blade 1, reducing the average particle size of the particles. In this manner, the apparatus of the present invention is notable in that by adjusting the vertical distance between the granulation part 1b of the stirring blade 1 and the fixed blade 2, granules having different average particle sizes can be obtained. It has characteristics. The only thing to be aware of is that if the fixed blade 2 is installed on an upward slope or if the length of the fixed blade 2 along the radial direction of the cylindrical container 4 is too large, the generation of swirling flow will be hindered and the particle layer will be It is to stagnate.
In order to avoid this, the length of the fixed blade 2 along the radial direction of the cylindrical container 4 must not be made larger than necessary. The granulation function of the particle processing device consisting of a combination of the fixed blade 2 and the stirring blade 1 has been explained above, but the fixed blade can also be replaced with a rotary blade 3 having a relative rotation direction opposite to that of the stirring blade 1. Similar granulation or particle processing functions can be exhibited. In other words, by setting the respective rotation speeds so that the relative rotation directions of the stirring blade 1 and the rotary blade 3 are opposite, the relative movement speed between the particles and the rotary blade 3 can be compared to when the fixed blade 2 is used. and become even bigger,
The crushing or grinding effect is further promoted. This helps reduce coarse particles, but on the other hand tends to make the particles irregularly shaped. Therefore, the relative rotation speed between the stirring blade 1 and the rotary blade 3 needs to be adjusted as appropriate depending on the particle size of the particles to be processed. Effects of the Invention When processing particles, a stirring blade having both an inclined surface that slopes downward in the direction of rotation and a substantially horizontal surface is attached to a rotating shaft supported at the center of a cylindrical container, and the stirring blade is is placed close to the bottom of the cylindrical container, and a fixed blade or a rotating blade is installed directly above the horizontal part of the stirring blade, and the particles flowing in the stirring direction during the granulation process are transferred to the fixed blade or rotating blade. In addition to impacting the particles by collision, the particles are sandwiched between the stirring blade and the fixed blade or the rotating blade, and coarse particles are crushed by the interaction between the stirring blade and the fixed blade or the rotating blade. By performing particle size distribution, the particle size distribution is uniform.
Moreover, granules with good sphericity can be obtained. As can be understood from the above explanation, by using the apparatus of the present invention, various problems observed in conventional granulated particle processing apparatuses can be solved, and particles with high sphericity and narrow particle size distribution can be produced. Moreover, spherical particles having a desired particle size can be efficiently produced. Implementation of the present invention provides many benefits. For example, when forming fine granules in the manufacturing process of pharmaceuticals, in order to keep the particle size distribution within an appropriate range, the granulated particles are sieved and divided into desired particle size ranges, and non-standard particles are collected. However, this is a major problem in fields such as pharmaceuticals, where content guarantees are strict and GMP is strongly required. However, according to the device of the present invention, most of the granulated product can be made into a product as is by simply removing a very small amount of coarse particles, which greatly simplifies the granulation operation and significantly improves productivity. do. Furthermore, when producing sustained release preparations, wax coating is applied to spherical particles to control elution of particle components. At this time, the higher the sphericity of the particles to be coated and the higher the smoothness of the particle surface, the more the dissolution is controlled according to the designed value. In this way, highly spherical granules with a diameter of 1 mm or less, which are required in the fields of "particle design" and "particle processing," for which the necessity has been actively voiced in recent years, can be efficiently produced by the apparatus of the present invention. . Thus, when the present invention is used as a granulation or coating means, it can improve the uniformity of sphericity and particle size distribution as well as bulk density in a wide range of fields of application ranging from pharmaceuticals to agrochemicals, foods, and ceramic products. brings notable benefits to

[Brief explanation of drawings]

FIG. 1 AB is a vertical cross-sectional view illustrating the overall structure of the device of the present invention, FIG. 2 is a vertical cross-sectional view illustrating different embodiments of the device of the present invention, and FIG. 3 is a plan view of the stirring blade. be. Figures 4A to G are diagrams illustrating the influence of the gap size between the fixed blade and the stirring blade on the particle size distribution of the granulated material, and Figure 5 illustrates the change in sphericity due to the interaction between the stirring blade and the fixed blade. line diagram,
FIG. 6 is a diagram illustrating the influence of the relative rotational speed of the rotary blade and the stirring blade on the particle size distribution. 1... Stirring blade, 1a... Inclined surface (swirling flow generation part),
1b...Horizontal part (granulating part), 2...Fixed blade, 3...Rotary blade, 4...Cylindrical container (stirring granulation tank), 5a, 5b
…Axis of rotation.

Claims (1)

[Claims] 1. Powder and a predetermined amount of liquid are put into a container, and the particles flowing in the stirring direction during the granulation process collide with a fixed blade or a rotating blade to apply an impact to the particles. The particles are sandwiched between the agitating blade and the fixed or rotating blade, and coarse particles are selectively crushed by the interaction between the stirring blade and the fixed or rotating blade, thereby regulating the particles. , adhesion, agglomeration,
A particle processing method characterized by performing rolling consolidation and crushing and grading in parallel. 2 In a particle processing device in which powder and a predetermined amount of liquid are put into a container and stirred by a stirring blade that rotates at high speed to adhere and bond the powder to form particles, a device supported at the center of a cylindrical container A stirring blade having both an inclined surface that slopes downward in the direction of rotation and a substantially horizontal surface is attached to the rotating shaft, and the stirring blade is disposed close to the bottom of the cylindrical container, and the horizontal surface of the stirring blade is A particle processing device characterized by having a fixed blade or a rotating blade installed directly above and close to the blade. 3. The particle processing device according to claim 2, wherein the fixed blade or the rotary blade is provided above the stirring blade and within a vertical distance of 1 to 20 mm. 4. The particle processing device according to claim 2, characterized in that the fixed blade is suspended from the top of the container, attached to the wall of the container, or supported and attached near the rotating shaft of the stirring blade. 5. Attach the rotary blade to the second rotating shaft supported by aligning the axis with the rotating shaft of the stirring blade, or
Claim 2, characterized in that the rotating blade is attached to a third rotating shaft suspended from the top of the container, and rotates in a direction opposite to the rotating direction of the stirring blade.
The particle processing device described in section.