JPH0618629B2 - Fluidized stirring granulation drying method and apparatus - Google Patents

Description

TECHNICAL FIELD The present invention relates to a granulating method and a granulating apparatus, and more particularly to a method and an apparatus for granulating using a fluidized bed.

SUMMARY OF THE INVENTION The present invention utilizes the shearing force of the granulating blades by injecting or spraying the binder into the granulating blades rotating at high speed in the fluidized bed. Even if the raw material has physical properties such that it cannot be granulated, it can be impacted, agglomerated, and sheared in a fluidized state to improve the granulation property. The target range of an object can be expanded.

Further, various effects such as the functions of mixing which is a pre-stage of granulation and drying which is a post-stage of granulation can be continuously performed in a single device are exhibited.

[Prior Art] Conventionally, as a granulation method, a so-called fluidized bed granulation method in which a powder is kept in a fluid state and a solution containing a binder is sprayed to perform agglomeration and granulation has been widely used.

This allows several steps, such as mixing-kneading-granulating-drying, which have been conventionally required, to be performed by the same device or machine, the number of steps can be reduced, and a short time in a sealed state can be achieved. Not only can it be performed, but there are various advantages such as rationalization of work, improvement of quality, and easy control of particle size.

However, with respect to the material to be granulated, for example, in the pharmaceutical industry or the like, granulation may not be possible unless the compression, shearing force, etc. are applied because of the wide range of physical properties of the raw material. For example, as an example thereof, a material having a hydrophobic physical property can be cited (as an example, an antibiotic powder can be cited). In the granulation of such physical properties as hydrophobic, unless a so-called high-speed stirring granulation method in which the powder and the binder are quantitatively supplied at the same time and the particles are agitated at high speed by a blade,
It cannot be granulated.

However, in such a stirring granulation method, the mixing (kneader and mixer may be required separately), kneading, and granulation in the previous step can be processed by the same device, but the drying step which is a post step. For that purpose, a dryer is required, and a structure for connecting and connecting each process is required, and it is unavoidable that the size is complicated and large as compared with the case of processing with a single device.

In the so-called dry granulation method, the solidified product is crushed, so that the product has an irregular shape, which is unsuitable for granulation of chemicals and the like.

[Problems to be Solved by the Invention] In the present invention, a series of steps of mixing-granulation-drying can be processed by a single apparatus, particle size control is easy, and the physical properties of the granulated material are influenced. It is an object of the present invention to obtain a method and an apparatus capable of granulating without causing any trouble.

[Means for Solving the Problems] In order to solve the above technical problem, the present invention forms a fluidized bed of powder in a gas phase and then rotates a granulation blade formed in the fluidized bed. . As a result, while further agitating the powder in the fluidized bed, the binder is injected or sprayed in the vicinity of the rotating granulation blade, and the binder is dispersed by the granulation blade, and at the same time, the granules are impacted and sheared. The composition is such that granulation is performed while adding.

[Operation] In the present invention, since the binder can be attached and aggregated in a fluidized state, the binder can be gradually added, and the progress of granulation (that is, particle size growth) is moderate, It becomes easy to control the particle size. Further, since the fluidized bed is used as in the fluidized bed granulation method, a series of steps of mixing-granulating-drying can be continuously performed in a single apparatus.

Furthermore, since the agglomeration by impact as well as the shearing force are used for granulation, not only the agglomeration by wetting as in the fluidized bed granulation method, granulation that is not affected by the physical properties of the granulated material is possible. is there.

[Embodiment] An embodiment of the present invention will be described below with reference to the drawings. However, it goes without saying that the components, other members and arrangements described or illustrated in the following explanation examples are
It is not intended to limit the present invention, but is merely an example of explanation.

FIG. 1 shows an embodiment of the present invention, FIG. 1 (A) is a side sectional view showing the outline of this embodiment, FIG. 1 (B) is a perspective view showing a granulating blade, and FIG. 1 (C). ) Is a cross-sectional view taken along line I-I of FIG. 1 (B).

In the figure, the fluidized bed forming apparatus S comprises a granulation chamber 1, an air supply duct 5, an exhaust duct 6, a dust collection chamber 10 equipped with a bag filter 4, and the like.

The granulation chamber 1 is composed of a cylindrical fluid tank 2 and a lower portion 3 having a truncated cone shape that is tapered downward from the fluid 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.

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 air flow straightening plate 7
Thus, the air supply duct 5 and the granulation chamber 1 of the fluidized bed forming apparatus S are defined.

A granulating blade 11 is provided in the granulating chamber 1, and the granulating blade 11 in this example has a disc-shaped bottom plate 11a and a donut-shaped upper plate 11b that are parallel to each other. 11b
The bottom plate 11a
Is fixed to the rotating shaft 12, and the rotating shaft 12 is connected to the motor 13
It is interlocked with. Any number of connecting pins 11c can be used depending on the purpose of the dispersing force of the binder and the shearing force for the powder or granular material.

A binder supply pipe 14 and a compressed air supply pipe 15 are arranged near the granulation blade 11 in this example. A preferable position of the binder supply pipe 14 is a position where the discharged binder is dispersed by the rotating granulation blade 11. Particularly in this example, the binder supply pipe 14 and the compressed air supply pipe 1 are provided in the central hole 11d provided in the donut-shaped upper plate 11b.
It is configured so that the end portion 5 is 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 the rotating shaft 22, and the rotating shaft 22 is connected to a motor. And granulation blade 2
The binder supply pipe 23 is positioned near the center of rotation of No. 1.

Even if it is configured as in this example, it is possible to obtain the same effect as that of the above-described example.

As described above, the shape of the granulating blade is not limited to a specific shape, and can be formed in any shape depending on the purpose such as the dispersing force of the binder or the powder, the impact force, or the like. Further, as to the attachment position of the binder supply pipe, as described above, it is not always required to be substantially at the center of the granulation blade, and it may be any position where the binder can be dispersed.

For example, the rotating shaft itself described in each of the above embodiments may also be used as the binder supply pipe. That is, as shown in FIG. 3, the side 31a in the rotation direction of the granulating blade 31 is replaced with the other side 31.
When it is set slightly higher than b and rotated, the powder flows as shown by the arrow. At this time, the binder supply pipe 3
When the tip 33 of No. 2 is formed so as to penetrate the granulation blade 31, even if the binder is discharged from the tip 33, the binder flows with the powder and the granulation can be performed.

In this way, by using the rotary shaft and the binder supply pipe in common, the piping and the like are facilitated, and the structure is simplified.

Next, the operation will be described.

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

Next, when the exhaust port damper 17 is opened and the exhaust fan 16 and the blower for air supply (not shown) are operated, air flows as shown by the solid line arrow in FIG. The body soars in the granulation chamber 1 and is fluidized. At this time, the air blown from the blower is configured to be warmed to a predetermined temperature by the heater 18.

When the granulating blade 11 is rotated while the powder is flowing in this way, the powder in the flowing state rotates.
Due to the centrifugal action of, the granules 11 flow from the center of rotation of the granulation blade 11 toward the outer peripheral direction. At this time, when the binder is injected or sprayed from the binder supply pipe 14, the binder is mixed with the powder along the flow of the powder and the granulation blade 11
Is vigorously dispersed by, mixed with powder and granulated into fine granules (primary mixing).

The finely granulated granules are discharged into the powder in the fluidized state, and the fluidized state is maintained again. Then, the powder particles that have been subjected to the primary mixing are again subjected to the granulation blade 11 similarly to the primary mixing.
Mixed by. At this time, granulation is further performed by the shearing force of the granulation blade 11. (Secondary mixing) In this granulation operation, the primary mixing and the secondary mixing are repeatedly carried out continuously, so that the particle size gradually increases, and the granulation can be continued up to the desired particle size. Will be easier.

As described above, in this example, not only the cohesive force due to mere wetting but also the cohesive force, the adhesive force, and the shear force by the granulating blade are used as the granulating elements, and the particle size can be easily controlled by these granulating elements. .

When the granulation reaches a desired particle size, injection (or spraying) of the binder and rotation of the granulation blade 11 are stopped. After this, leave the blower 16 and blower running,
Move to a step for drying. In the drying process, the heater 18 is adjusted so as to reach a predetermined temperature.

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

An example according to the invention is given below.

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

Specific volume: Loose value: 1.50 ml / g Pat value: 1.32 ml / g Angle of repose: 35 ° Moisture value: 0.4% Particle size distribution is a No. 16-200 standard size sieve with a yield of 8
It was 9.1%.

This result indicates that the specific volume of the granulated granules obtained from the same kind of raw material in the conventional example has a loose value of 2.0 ml / g, so that the present invention is heavier than the conventional one.

Also, the amount of binder used (liquid content) relative to the amount of raw material powder
In comparison with the conventional fluidized-bed granulator, the particle size grew to a desired particle size by about half the amount, and it became possible to reduce the amount of binder and shorten the drying time.

[Example 2] 6 kg of granulated and pulverized powder containing a drug substance was charged into the apparatus according to the present invention, and 3.75 kg of water was gradually added to granulate. Then, it was fluidized and dried in the same apparatus to obtain granulated granules. The granulated granules have a viscosity distribution of 8 to 100 on a No. 20-200 standard sieve.
It was 9.2%.

Granulation with a fluidized granulator using conventional raw materials of the same type has been impossible because of the raw material characteristics (hydrophobicity).

[Advantages of the Invention] The present invention, which is configured as described above, has the following advantages.

According to the present invention, in a fluid state, adhesion by a binder,
Since the agglomeration can be performed, the binder can be gradually added, the progress of granulation (that is, the growth of the particle size) is moderate, and the particle size control becomes easy. Further, since the fluidized bed is used as in the fluidized bed granulation method, a series of steps of mixing-granulation-drying can be continuously performed in a single apparatus.

Furthermore, since the agglomeration by impact as well as the shearing force are used for granulation, not only the agglomeration by wetting as in the fluidized bed granulation method, granulation that is not affected by the physical properties of the granulated material is possible. is there.

[Brief description of drawings]

FIG. 1 shows an embodiment of the present invention, FIG. 1 (A) is a side sectional view showing the outline of this embodiment, FIG. 1 (B) is a perspective view showing a granulating blade, and FIG. 1 (C). ) Is a cross-sectional view taken along the line I-I of FIG. 1 (B), and FIGS. 2 and 3 are perspective views showing another embodiment of the granulating blade. 1 ... Granulation chamber, 4 ... Filter, 5 ... Air supply duct, 6 ... Exhaust duct, 10 ... Dust collection chamber 11, 21, 31 ... Granulation blade, 12 ... Rotation shaft, 14, 23 ... Binder supply pipe.

Claims (5)

[Claims] 1. A rotating granulating blade and a binder supply pipe in the vicinity of the granulating blade are disposed at least inside a fluidized bed of a fluidized bed forming apparatus to accommodate powder to be granulated, After forming a fluidized bed of the powder, by rotating the granulating blade, while further stirring motion of the powder in the fluidized bed, injecting or spraying a binder in the vicinity of the rotating granulating blade, A fluidized agitation granulating and drying method characterized in that a binder is dispersed by a granulating blade, and granules are granulated while being impacted and sheared. 2. The fluidized agitation granulation drying method according to claim 1, wherein the granulation blade is rotated at a high speed. 3. A fluidized bed forming apparatus having at least a granulating chamber for suspending powder in a gas phase, wherein a rotating granulating blade arranged in the granulating chamber and a granulating blade in proximity to the rotating granulating blade. A fluidized agitation granulating / drying device comprising a binder supply pipe provided as described above. 4. The fluidized agitation granulating / drying apparatus according to claim 3, wherein the granulating blade rotates at a high speed. 5. The fluidized agitation granulating / drying apparatus according to claim 3, wherein the binder supply pipe is integrated with a rotary shaft.