JPH0741154B2 - Spray cooling granulation method and apparatus - Google Patents

Description

TECHNICAL FIELD The present invention relates to a spray cooling granulation method and apparatus, and in particular, a spray cooling granulation chamber (hereinafter referred to as a granulation chamber) formed of a porous film. The present invention relates to a granulation method and apparatus.

[Conventional technology]

The spray cooling granulation method and apparatus basically consist of spraying the stock solution,
It has three essential functions: cooling of sprayed microdroplets and separation / collection of powder / granular products. Normally, spray cooling granulators have a sprayer, a granulating chamber and a powder / granular material recovery system. Equipped with a vessel.

Conventionally, as an example of such a spray cooling granulating apparatus, those shown in FIGS. 6, 7, and 8 are known.

In the spray cooling granulator of FIG. 6, in the granulation chamber 1,
The stock solution sprayed from the nozzle 5 is instantaneously cooled by the cold air blown from the inlet 2, and the liquid component is solidified,
It is made into powder. Most of the powdery particles are taken out as a product through the rotary valve 6, but a part of the powdery particles is entrained by the cold air and passed through the exhaust port 3 to be collected from the rotary valve 8 in the cyclone 7.

FIG. 7 shows a spray cooling granulator of the type in which spray and cold air flow in countercurrent.

The spray cooling granulator of FIG. 8 is of a type in which a rotary spray disk 10 is used as a sprayer instead of the nozzle 5.

Of these, in the spray cooling granulator of the type shown in FIGS. 6 and 7, as described above, the product particles are collected separately from the main body of the device and the cyclone. Is a cyclone, and the one with a relatively large weight and a large particle size is taken out from the main body of the apparatus, and a minute composition separation occurs in the product.

On the other hand, the device of the type shown in FIG. 8 is mainly used as a manufacturing device for pharmaceutical products, and the product granules are cyclone 7
Although it is recovered only by itself, the differential powder product containing useful components is scattered to the back filter 16 and the like, causing contamination and composition separation.

In the past, this composition separation did not pose a problem depending on the type of product.

By the way, recently, as for the spray cooling granulation method and apparatus, a multi-product small-quantity production system for pharmaceuticals, fine chemicals, etc. has been demanded from a conventional small-product mass production system.

In addition, the number of cases in which higher-purity products are required as products has increased.

[Problems to be solved by the invention]

As described above, the demand for a high-mix low-volume production method and the production of high-purity products has brought about new problems in addition to the above-mentioned composition separation, which has hardly been a problem in the conventional case.

In other words, due to the frequent switching of product types, it has become necessary to quickly and completely wash the adhered solids on the inner wall of the granulation chamber. Because
It takes a fatal defect to take a long time for cleaning in order to efficiently perform high-mix low-volume production, and when high purity and high quality are required for product quality, the adhered solid content is completely removed when changing product types. Cleaning is necessary, but in reality, complete cleaning is extremely difficult. In addition, if the product is harmful to the human body, it cannot be directly touched and cleaning is extremely difficult.

In addition, the minute composition separation as described above has also become a problem due to the demand for high-purity products.

[Means for solving problems]

In view of the above-mentioned problems of the prior art, the inventors of the present invention have conducted extensive studies, and as a result, found that the above problems can be solved by forming the granulation chamber with a porous film, and arrived at the present invention. .

That is, according to the present invention, in a spray cooling granulation method of spraying a molten undiluted solution into fine liquid droplets and cooling it to immediately produce powder from the undiluted solution, the granulation chamber has a bag-like or cylindrical shape. A spray-cooling granulation method is provided, which is formed of a good peeling porous film, and the exhaust gas and the powder are immediately separated by the porous film to obtain the total amount of the powder from the granulation chamber.

Further, according to the present invention, in a spray cooling granulating apparatus in which a molten stock solution is sprayed on fine liquid droplets and cooled to produce a powder immediately from the stock solution, the granulating chamber has a bag-like or cylindrical shape. Provided is a spray-cooled granulation device formed of a peelable porous film.

The stock solution spray-granulated in the present invention, for example, a wax or a hot-melt resin, is a liquid at a certain temperature or higher, a solid substance at a certain temperature or lower, and a small amount of an additive component such as a drug or a fragrance. A liquid obtained by heating and melting a substance added with is used.

The porous membrane used in the present invention must be disposed in the spray cooling granulator main body and have excellent releasability.

That is, the temperature of the cold air introduced into the granulation chamber is usually 0 to 40 ° C at the inlet and 15 to 60 ° C at the outlet, so it must withstand these temperatures, and the fine powder always adheres. However, since it is deposited, it must have good peelability for continuous use. Further, this porous membrane separates the target product fine powder from gas.

The type of the porous membrane having such a function is not particularly limited, but usually a cloth made of fiber or a combination membrane in which two or more kinds thereof are combined is used. As a preferable porous membrane, a well-removable mesh membrane to which a woven or non-woven fabric as a strength material is laminated is used. In this case, specifically, the mesh membrane is polytetrafluoroethylene (PT).
FE) (trade name Teflon) type membrane, polytrifluoroethylene type membrane, woven cloth, non-woven cloth, nylon, polyethylene,
Those made of polyester or cotton cloth are preferably used.

Further, in the present invention, the entire granulation chamber is formed of a single porous membrane, which is easy to remove from the device, and therefore its maintenance is extremely simple.

[Action]

The undiluted solution sprayed in the bag-shaped or cylindrical granulation chamber made of a porous film arranged in the spray cooling granulator main body is instantaneously cooled by cold air with an inlet gas temperature of 0 to 40 ° C blown from the inlet. It is cooled and solidified into gas and powder. The powder and granules largely settle at the bottom of the granulation chamber due to their own weight, while the gas is separated from the remaining powder and granules through the ventilation holes of the porous membrane and the exhaust port 3
It is exhausted to the outside through the. Therefore, since all the powder and granules are separated from the gas by the porous film, the composition separation of the product powder and granules does not occur.

Further, if the continuous operation is performed, the granular material adheres to and accumulates on the porous membrane, the pressure loss increases, and the operation must be stopped at last, so that the granular material must be appropriately blown off. At that time, since the granulation chamber is formed of a bag-like or tubular porous film with good releasability, the adhered powdery particles are shorted by mechanical vibration or by air injection (pulse air) from the opposite side. You can easily get rid of it in time. Also,
At that time, in order to completely clean and prevent mixing of impurities, it is performed from the outside without touching the internal product by replacing the porous membrane, but it is easy to replace because it is a single bag-shaped Is.

Further, the separation of the powder and granules from the gas by the porous membrane is usually carried out by passing the gas containing the powder and granules through the cloth of the fibers constituting the porous membrane to filter out only the fine particles therein. However, in practice it is not a simple filtration, and the texture is usually many times larger than the particles to be separated. Therefore, the powdery particles are not only collected on the surface of the filter cloth but also inside thereof to be collected. In the case of the present invention, such a filter cloth is mainly used for powders and granules which are easily soluble in a solvent. However, it is desirable to use a combination film of the woven or non-woven fabric, which has good releasability with respect to the granular material and which has the network film on the surface of which surface filtration is performed and which has excellent strength. Increase the effect more. Then, the range of the separable particle size of the porous membrane extends over a wide range from 0.1 μm to several mm.

〔Example〕

Next, the present invention will be described in more detail based on the embodiments shown in the accompanying drawings.

FIG. 1 shows an embodiment of an apparatus using the spray cooling granulation method according to the present invention. (A) is a schematic sectional view of the entire apparatus, (b) is a porous membrane forming a granulation chamber. FIG. In the figure, inside the spray cooling granulator main body 11, the granulation chamber 1 formed of a bag-shaped porous film 15 is arranged along the inside thereof. As shown in FIG. 1B, this porous membrane 15 has a mesh membrane 13 and a filter cloth 14 which is a strength material.
It is made up of glued together. The cold air X _C is fed downward from the upper part of the apparatus main body 11 into the granulation chamber 1 through the inlet 2, and is sprayed upward from the lower center of the granulation chamber 1 through the nozzle 5. In countercurrent contact with. The product powder and granules enter the product receiver 17 from the outlet 6 by the seal valve, and the gas is separated from the powder and granules A through the porous membrane 15 forming the outer wall of the granulation chamber, and is exhausted as Y, respectively. Is discharged to.

FIG. 2 is a schematic cross-sectional view showing another embodiment of the present invention, in which a rotating atomizing disc 10 is used as the atomizing device instead of the nozzle 5, and the cold air X _C is spread downward from the nebulizing liquid from the atomizing disc 10. It differs from FIG. 1 in that it is introduced by a flow, and hot air X _H is introduced from around the atomizing disk 10. Accordingly, when a liquid having a high temperature dependency of viscosity is sprayed, for example, a liquid such as petroleum wax that solidifies and becomes a filament before being atomized and atomized can be spheroidized. When it becomes a filament, it becomes a cotton candy-like production device, not a granulation device for powder.

3 to 5 are also schematic cross-sectional views showing other embodiments of the present invention. FIG. 3 shows the cold air X _C and the undiluted solution from the nozzle 5 being introduced in a downward parallel flow. Figure 4 shows cold wind X _C
And the undiluted solution from the nozzle 5 is introduced in a parallel flow upward, and FIGS. 5 (a) and 5 (b) show that the cold air X _C and the undiluted solution from the nozzle 5 are introduced from the lateral direction. .

The apparatus shown in FIGS. 3 to 5 is provided with a brushing-off mechanism (backwashing type, pulse air type) Z for brushing off the granular material. For example, pulse air is passed through the line 12. The particles A fed into the apparatus main body 11 from the opposite direction and attached to the porous film 15 are wiped off.

Hereinafter, the spray cooling granulation method and apparatus of the present invention will be described more specifically.

(Example 1) Using a spray cooling granulating apparatus of the type shown in FIG. 1, 97 wt% of beeswax exposed as cooling granulation target, 3 wt% of chlorotetracycline as drug, 97 wt% of beef tallow and 3 wt% of penicillin as drug , 2 types, throughput 100kg / Hr
Was sprayed. The granulation chamber has a diameter of 2500 mm and a straight body height of 2500.
mm, total height 4300 mm, the upper part was cylindrical, and the lower part was funnel-shaped. As the porous film forming the granulation chamber, a combination film obtained by laminating polytetrafluoroethylene on polyethylene nonwoven fabric was used. The cold air inlet temperature was 15 ° C, and the exhaust air temperature was 30 ° C.

The stock solution was spray-dried under the above conditions. As a result, the properties of the product granules were as follows.

(1) (2) Product particle size (average) 140μm 120μm Product temperature 40 ° C 35 ° C Composition variation None None Yield after 4 hours operation 99% 99% Note that (1) is a chlorotetracycline preparation and (2) is penicillin. The formulation is shown.

When switching products, the time required for switching is approximately 40
It took only a minute.

〔The invention's effect〕

As described above, since the granulation chamber of the spray cooling granulation apparatus of the present invention is formed of a porous film, fine powder having a small particle size is accompanied by gas and discharged to the outside of the apparatus main body as in the conventional case. Since there is no compositional separation, it is possible to quickly and easily wash and remove the adhered fine powder even when frequent product types are changed due to the multi-product small-quantity production method. Higher quality and higher purity are possible.

Further, there is an effect that a dust collecting device which has conventionally been separately installed is unnecessary.

[Brief description of drawings]

FIG. 1 shows an embodiment of the spray cooling granulating apparatus according to the present invention. (A) is a schematic sectional view of the entire apparatus, (b) is a partially enlarged sectional explanatory view of a porous membrane, and FIG. FIG. 5 to FIG. 5 are schematic sectional views showing other embodiments of the present invention, and FIG. 6 to FIG.
The figure is a schematic cross-sectional view showing a conventional spray cooling granulator. 1 ... Granulation chamber, 2 ... Cold air inlet, 3 ... Exhaust outlet, 5 ...
Nozzle, 6 ... Product outlet, 7 ... Cyclone, 10 ... Spray disc, 11 ... Device body, 13 ... Mesh membrane, 14 ... Filter cloth, 15 ... Porous membrane, 16 ... Bag filter , 17 ……
Product receiver, X _C ... Cold air, X _H ... Hot air, Y ... Exhaust air, Z ...
… Shedding mechanism.

 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Hiroki Takahashi 1-13-1, Nihonbashi, Chuo-ku, Tokyo TDC Inc. (72) Inventor Masaaki Okawara 3847 Ikebecho, Midori-ku, Yokohama-shi, Kanagawa Okawara Kakoki Co., Ltd. Co., Ltd. (72) Inventor Katsumi Kobayashi 3847 Ikebe-cho, Midori-ku, Yokohama-shi, Kanagawa Okawara Kako Kikai Co., Ltd.

Claims (5)

[Claims] 1. A spray cooling granulation method in which a molten stock solution is sprayed into fine droplets and cooled to immediately produce a powder from the stock solution. In the spray cooling granulation chamber, the spray cooling granulation chamber has a bag-like or cylindrical shape. A spray cooling granulation method characterized in that it is formed of a peelable porous film, and the cooling exhaust gas and the powder are immediately separated by the porous film to obtain the total amount of the powder from the spray cooling granulation chamber. . 2. The spray-cooled granulation according to claim 1, wherein the porous membrane is a combination membrane of a mesh surface filtration membrane having good releasability from powder and a filter cloth as a strength material. Method. 3. The spray cooling granulation method according to claim 1, wherein hot gas having a temperature higher than the melting point of the stock solution is blown into the spray cooling granulation chamber from the periphery of the spray stock solution. 4. In a spray cooling granulating apparatus for spraying a molten stock solution into fine droplets and immediately cooling the stock solution to produce a powder, the spray cooling granulation chamber has a bag-like or cylindrical shape. A spray-cooling granulating apparatus characterized by being formed of a peelable porous film. 5. The spray cooling granulation according to claim 4, wherein the porous membrane is a combination membrane of a mesh surface filtration membrane having a good releasability from powder and a filter cloth as a strength material. apparatus.