JPS62258733A - Method and apparatus for fluidized stirring granulation and drying - Google Patents

Abstract

PURPOSE:To make a granulation speed moderate and to facilitate the control of a particle size, by a method wherein a binder is injected or sprayed in the vicinity of a rotating granulation blade and dispersed in a substance to be granulated while an impact and shearing are applied to said substance to perform granulation. CONSTITUTION:When an exhaust port damper 17 is opened and an exhaust fan 16 and a blower are operated, air flows as shown by an arrow and a powder is blown up and fluidized in a granulation chamber 1. If a granulation blade 11 is rotated in this state, the powder flows from the rotary center part to the outer peripheral direction by the centrifugal action of the granulation blade 11. When a binder is injected or sprayed from a binder supply pipe 14 at this time, the binder is mixed with the powder while moved along the flow of the powder and violently dispersed by the granulation blade 11 and further mixed with the powder to granulate said powder into a fine granule. This granule is discharged in the powder held to a fluidized state to again hold the fluidized state.

Description

DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a granulation method and a granulation device, and more particularly to a granulation method using a wave bed and its device.

[Summary of the Invention] The present invention utilizes the tube shearing force of the granulation blades by injecting or spraying the binder into the granulation blades rotating at high speed within the fluidized bed, so it is not possible to use conventional fluidized bed granulation. Even if the raw material has physical properties that cannot be granulated by this method, it can be granulated in a fluid state.
It becomes possible to apply impact, agglomeration, and shearing, improve granulation properties, and expand the target range of granulated materials without worrying about the physical properties of the granulated materials.

In addition, it has various effects in that the functions of mixing, which is the pre-stage of granulation, and drying, which is the post-stage, can be performed continuously in a single device.

[Prior Art] Conventionally, the so-called fluidized bed granulation method, in which powder is kept in a fluid state and a solution containing a binder is sprayed onto it to form agglomerated particles, has been widely used. There is.

This allows several steps that were previously required, such as mixing, coalescence, granulation, and drying, to be performed in the same device or machine, reducing the number of steps and allowing the process to be completed in a short period of time under closed conditions. This is because there are various advantages such as streamlining of work, improvement of quality, and easy control of particle size.

However, regarding materials to be granulated, for example, in pharmaceutical products, etc., the physical properties of the raw materials vary widely, so granulation may not be possible without applying compression, shearing force, etc. (An example is antibiotic powder). When granulating materials with hydrophobic physical properties, it is impossible to granulate them unless the so-called high-speed agitation granulation method is used, in which powder and binder are simultaneously supplied in fixed amounts and agitated at high speed using blades. I can't.

However, this type of stirring granulation method requires the mixing (
(In some cases, a separate mixer may be required), kneading, and granulation can be processed using the same equipment, but a dryer is required for the subsequent drying process, which requires the connection and granulation of each process.
A continuous structure is required, and it is inevitable that the process will be more complicated and larger than when processing with a single device.

Furthermore, in the so-called dry granulation method, the combined solids are crushed, resulting in an irregularly shaped product, which is unsuitable for granulation of drugs and the like.

[Problems to be solved by the invention] The present invention can process a series of steps of mixing, granulation, and drying with a single device, and can easily control the particle size, which is dependent on the physical properties of the material to be granulated. The object of the present invention is to provide a method and device that can perform granulation without causing any problems.

[Means for Solving the Problems] In order to solve the above-mentioned technical problems, the present invention involves forming a fluidized bed of powder in a gas phase, and then rotating granulation blades formed in the fluidized bed. . As a result, while further stirring the powder in the fluidized bed, the binder is injected or sprayed near the rotating granulation blades, and the binder is dispersed by the granulation blades while at the same time impacting the material to be granulated. The structure is such that granulation is performed while applying shear.

[Function] The present invention allows adhesion and aggregation by the binder in a fluid state, so the binder can be added gradually, and the progress of granulation (that is, the rate of particle size growth) is slow. , particle size control becomes easy. In addition, since a fluidized bed is used in the same way as the fluidized bed granulation method, mixing, granulation, and
A series of drying steps can be performed continuously.

Furthermore, for granulation, it uses not only agglomeration due to moisture as in the fluidized bed granulation method, but also agglomeration due to impact and shearing force, so granulation can be performed without being affected by the physical properties of the material to be granulated. be.

[Example] An example of the present invention will be described below with reference to one drawing. However, it should be noted that the components, other members, ff, and locations described or illustrated in the following illustrative examples are not intended to limit the present invention, but are merely illustrative examples.

FIG. 1 shows an embodiment of the present invention, FIG. 1(A) is a side sectional view schematically showing this example, FIG. 1(B) is a perspective view showing a granulating blade, and FIG. ) is a sectional view taken along the line I-I in FIG. 1(B). In FIG. It consists of a dust collection chamber 10 etc. equipped with 4.

The granulation chamber 1 consists of a cylindrical fluidized tank 2 and a truncated conical lower part 3 that tapers downward from the fluidized tank 2. A bag filter 4 is disposed above the granulation chamber 1, and the bag filter 4 defines the granulation chamber 1 and a dust collection chamber 10 to which an exhaust duct 6 is connected. .

Further, an air supply duct 5 is connected to the bottom of the granulation chamber 1, and an air flow rectifying plate 7 made of a perforated plate is arranged between the granulation chamber 1 and the air supply duct 5. This airflow rectifier plate 7
The air supply duct 5 and the granulation chamber l of the flow layer forming device S
is defined.

A granulation blade 11 is provided in the granulation chamber 1, and the granulation blade 11 in this example has a disk-shaped bottom plate 11a and a donut-shaped top plate 11b as parallel surfaces. 11b
are combined with a connecting bottle 1ice..., and the bottom plate 11
a is fixed to the rotation shaft 12, and the rotation shaft 12 is connected to the motor 1.
It is linked to 3. Note that any number of connecting pins llc can be used depending on the purpose of the dispersion force of the binder and the shearing force for the powder or granular material.

In this example, a binder supply pipe 14 and a compressed air supply pipe 15 are arranged near the granulation blade 11.

A preferable position of the binder supply pipe 14 is a position where the discharged binder is dispersed by the rotating granulation blades 11. In particular, in this example, the binder supply pipe 14 is preferably placed in the central hole lid provided in the donut-shaped upper plate 11b. It is configured such that the ends of the binder supply pipe 14 and the compressed air supply pipe 15 are located.

In this example, a normal binder supply pipe is used, but a spray nozzle may be used to improve the dispersion of the binder.Furthermore, although a compressed air supply pipe is provided in this example, It can be omitted if the binder can be sufficiently stirred, such as when using a spray nozzle.

FIG. 2 is a perspective view showing another embodiment of the granulating blade.

In this example, the granulating blade 21 is formed into a cross-shaped flat plate, the blade 21 is fixed to a rotating shaft 22, and the rotating shaft 22 is connected to a motor.

Then, the binder supply pipe 23 is located near the rotation center of the granulating blade 21.

Even if configured as in this example, the same effects as in the above embodiment can be achieved.

As described above, the shape of the granulating blade is not limited to a specific shape, and can be formed into any shape depending on the purpose of dispersing the binder, powder, etc., impact force, etc. Furthermore, as for the location of the binder supply pipe, as mentioned above, it does not necessarily have to be located approximately at the center of the granulating blades, but may be at any location where the binder can be dispersed.

For example, the rotating shaft itself explained in each of the above embodiments may also be used as the binder supply pipe, that is, as shown in FIG.
If it is made slightly higher than b and rotated, the powder will flow as shown by the arrow. At this time, binder supply pipe 3
If the tip 33 of the powder is formed so as to pass through the granulation blade 31, even if the binder is discharged from the tip 33, the binder will flow together with the flow of the powder and granulation can be performed.゛By using the rotary shaft and the binder supply pipe in this way, piping etc. become easy and the structure becomes simple.

Next, the effect will be explained.

First, from the material supply port (not shown) of the fluidized bed forming apparatus S,
A powder material is put into the granulation chamber 1, and the material supply port is closed.

Next, when the exhaust port damper 17 is opened and the exhaust fan 16 and the air supply blower (not shown) are operated, FIG.
) Air flows as shown by the solid arrow, and the powder flies up into the granulation chamber 1 and becomes fluidized. At this time, the air coming out of the blower is configured to be heated to a predetermined temperature by the heater 18.

With the powder flowing in this way, the granulating blades 7141
1, the fluidized powder flows from the center of rotation of the granulating blades 11 toward the outer circumference due to the centrifugal action of the rotating granulating blades 11. At this time, when the binder is injected or injected from the binder supply pipe 14, the binder flows along the flow of the powder.

While being mixed with the powder, it is well dispersed by the granulating blades 11, and further mixed with the powder and granulated into fine granules (secondary mixing).

The finely granulated granules are discharged into the fluidized powder, and the fluidized state is maintained again. and.

Furthermore, the powder and granules mixed in the -th stage are
Mixing is carried out by the slot granulating blades 11. At this time, granulation is further performed by the shearing force of the granulation blades 11. (Secondary mixing) In this granulation action, secondary mixing and secondary mixing are repeated and repeated, so the particle size gradually increases and granulation can be continued until the desired particle size is reached. Control becomes easier.

- As mentioned above, in this example, not only the cohesive force due to wetting, but also the cohesive and adhesive force due to the granulation blades.

Shearing force is also used as a granulation factor, and these granulation factors make it easy to control particle size.

When the granulation reaches the desired particle size, binder injection (
or Funikichi) and the rotation of the granulation blade 11 is stopped. After this, the exhaust fan 16 and the blower remain in operation, and the process moves to drying. In the drying process, the heater 18 is adjusted to maintain a predetermined temperature.

In this way, after the predetermined time for drying has passed,
After the granulated granules are generated, when the exhaust port damper 17 is closed, the granulated granules fall and are deposited on the current plate 7, and the series of process operations is completed.

Examples according to the invention are listed below.

[Example 1] 12 kg of lactose was charged into the apparatus according to the above example, and HP
1.8 kg of C-5L 8% aqueous solution was gradually added and granulated. Thereafter, it was fluidized and dried in the same apparatus to obtain granules. Granulated granules are as follows.

Specific volume is loose value: t, 50m sentence/g putt value:
1.32 mb/g Angle of repose: 35° Moisture value: 0.4% Particle size distribution is a pharmacopoeia standard sieve of No. 16 to No. 200, yield is 8
It was 9.1%.

This result shows that the specific volume of the granules obtained using the same kind of raw material as in the conventional example was a loose value of 2.0 mft/g, and therefore the present invention was heavier than the conventional example.

In addition, the amount of binder used (liquid content) for the raw material powder can be grown to the desired particle size in about half the time compared to conventional fluidized granulation equipment, reducing the amount of binder and shortening drying time. It has become possible.

[Example 1 2] 6 kg of granulated pulverized powder containing a pharmaceutical active ingredient was charged into the apparatus according to the present invention, and 3.75 kg of water was gradually added thereto for granulation. Thereafter, it was fluidized and dried in the same apparatus to obtain granules. The particle size distribution of the granules was sieved using a No. 20 to No. 200 Japanese Pharmacopoeia standard sieve, and the yield was 83.2%.

Conventional granulation using a fluidized granulator using the same type of raw material was not possible due to the raw material characteristics (hydrophobicity).

[Effects of the Invention] Since the present invention is configured as described above, it has the following effects.

According to the invention, in a fluid state, attachment by a binder,
Since aggregation can be carried out, the binder can be added gradually, the rate of granulation progress (that is, the growth of the particle size) is slow, and the particle size can be easily controlled.

Further, since a fluidized bed is used as in the fluidized bed granulation method, a series of steps of mixing, granulation, and drying can be performed continuously in a single device.

Furthermore, for granulation, it uses not only agglomeration due to moisture as in the fluidized bed granulation method, but also agglomeration due to impact and shearing force, so granulation can be performed without being affected by the physical properties of the material to be granulated. be.

[Brief explanation of drawings]

FIG. 1 shows an embodiment of the present invention, FIG. 1(A) is a side sectional view schematically showing this example, FIG. 1(B) is a perspective view showing a granulating blade, and FIG. ) is a sectional view taken along line II in FIG. 1 CB), and FIG. 2 is a perspective view showing another embodiment of the granulation blade. l... Granulation chamber, 4... Filter, 5...
Supply air duct, 6... Exhaust duct, 10... Dust collection chamber, 11, 21. 31... Granulation vane. 12...Rotating shaft, 14.23...Binder supply pipe. Patent applicant: Yamanouchi Pharmaceutical Co., Ltd. Figure 2 Figure 3 Procedural amendment (method) 1. Display of the case 1985 Patent Application No. 283543 2 Name of the invention Fluidized agitation granulation drying method and its apparatus 3 Person making the amendment Relationship to the case Patent applicant Representative Shigeo Morioka 4, Agent

Claims (1)

[Claims] 1. At least inside the fluidized bed of the fluidized bed forming device, a rotating granulation blade and a binder supply pipe are provided in close proximity to the granulation blade, and the powder to be granulated is After accommodating the powder and forming a fluidized bed with the powder, the powder in the fluidized bed is further stirred by rotating the granulation blade, while
Injecting or spraying a binder near the rotating granulation blades,
A fluidized agitation granulation drying method characterized by dispersing a binder with granulation blades and granulating the material while applying impact and shear to the material to be granulated. 2. The fluidized agitation granulation and drying method according to claim 1, characterized in that the granulation blades are rotated at high speed. 3. In a fluidized bed forming apparatus equipped with a granulation chamber in which at least powder is suspended in a gas phase, a rotating granulation blade disposed within the granulation chamber and a rotating granulation blade provided close to the granulation blade are provided. 1. A fluidized agitation granulation drying device characterized by comprising a binder supply pipe and a binder supply pipe. 4. The fluidized agitation granulation drying apparatus according to claim 3, wherein the granulation blades rotate at high speed. 5. The fluidized agitation granulation drying apparatus according to claim 3 or 4, wherein the binder supply pipe is integrated with a rotating shaft.