JPH1025304A - Method for granulating powder consisting of a substance ingested into animal body and granulated material - Google Patents

Abstract

(57) [Problem] To provide an industrial granulation method which can be advantageously applied to powder of a substance to be taken into an animal body. SOLUTION: In a method of granulating a powder of a substance to be taken into the body of an animal into a granule having an average particle diameter of 100 to 1500 μm, at least a part of the powder is formed by an ascending airflow through a gas dispersion plate. A spray liquid composed of an aqueous solution of hemicellulose is sprayed as fine droplet particles through a spray nozzle onto a powder fluidized bed formed by fluidization, and a plurality of powder particles are sprayed in the presence of the fine droplet particles of the spray liquid. A granulation step of adhering and bonding the particles to each other to form a granulated product, wherein the viscosity of the spray liquid is in the range of 3 to 100 mpa · s, and the fine droplet particle diameter of the spray liquid formed by spraying from the spray nozzle Is in the range of 10 to 200 μm, and the content of particulate matter in the particle size range of 0.7 M to 1.3 M (where M is the average particle size of the granulated material) in the obtained granules is 75. Weight percent or more It said method characterized by.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for granulating a powder of a substance to be ingested into the body of an animal and a granulated product.

[0002]

2. Description of the Related Art Granulation of powders in the presence of a binder is widely performed for improving the handleability of the powders and for combining a plurality of powders. In such a method of granulating powder, when the powder is composed of a substance to be ingested into an animal body including a human, such as a food or a pharmaceutical, the binder is highly safe for animals. Is required. In this case, it is also an important factor that the binder has high binding properties and low cost. On the other hand, a granulated product obtained by granulating a powder is required to have as sharp a particle size distribution as possible from the viewpoint of its use characteristics. Conventionally, as a method of granulating powder, various methods including the type of binder are known, but when granulating powdery foods or pharmaceuticals,
From the viewpoint of safety, there is still no satisfactory method because there is a great restriction on the selection of the binder, and there is no industrially advantageous method that can efficiently obtain granules having a sharp particle size distribution. The development of a granulation method is desired.

[0003]

SUMMARY OF THE INVENTION An object of the present invention is to provide an industrial granulation method which can be advantageously applied to a powder of a substance to be taken into an animal body.

[0004]

Means for Solving the Problems The present inventors have conducted intensive studies to solve the above-mentioned problems, and as a result, have completed the present invention. That is, according to the present invention, in a method of granulating a powder of a substance to be taken into the body of an animal into a particulate having an average particle diameter of 100 to 1500 μm, at least a part of the powder is passed through a gas dispersion plate. A spray liquid composed of an aqueous solution of hemicellulose is sprayed as fine droplet particles through a spray nozzle onto a powder fluidized bed formed by fluidization by the raised airflow, and a plurality of spray liquids are formed in the presence of the fine droplet particles of the spray liquid. Wherein the spray liquid has a viscosity in the range of 3 to 100 mPa · s, and the fine particles of the spray liquid formed by spraying from the spray nozzle are included. Droplet particle size is 10 to 200 μm
In addition, 0.7M in the resulting granulation ~
The above-mentioned method is provided, wherein the content of the particulate matter in the particle size range of 1.3 M (where M is the average particle diameter of the granulated substance) is 75% by weight or more.

[0005]

BEST MODE FOR CARRYING OUT THE INVENTION The raw material to be treated used in the present invention is a powder of a substance to be ingested into an animal body. Such a powder includes edible substances, physiologically active substances, and additives to these substances. Agents and the like. Edible substances include carbohydrates, proteins and fats. Specific examples of edible substances include starch, sucrose, maltose,
Dextrin, flour, protein, peptide, amino acid,
Examples include agar, vegetable fiber, coffee, tea, cocoa, health foods, seasonings, spices, feeds, and the like. Bioactive substances include pharmaceuticals, vitamins, calcium salts, chlorella,
Bifidobacterium, ginkgo biloba extract and the like. Also,
Additives include colorants, preservatives, extenders and the like. Powders are broadly classified into self-binding powders and non-self-binding powders, which are attached by water or an organic solvent, and the granulation method of the present invention uses any of these powders. The same can be applied. The average particle size of the powder is usually 200 μm.
m, preferably 10 to 100 μm.

[0006] The granulating binder used in the present invention is water-soluble hemicellulose and is a conventionally known substance. This water-soluble hemicellulose is obtained by hydrolyzing a water-insoluble plant fiber composed of a polysaccharide present in a plant body by binding to cellulose or the like under weak acidity and separating a water-soluble product. Can be. As the water-insoluble plant fiber, a water-insoluble plant fiber of oil seeds such as soybean and palm palm and a water-insoluble plant fiber of cereals such as rice, wheat and corn are used. Okara obtained after removing most of it can be used advantageously. The hydrolysis reaction of the water-insoluble plant fiber needs to be performed under a pH condition near the isoelectric point of the protein contained in the water-insoluble plant fiber. When the raw material is okara, the hydrolysis reaction is performed at pH 3 to 7, preferably 4 to 7, since the isoelectric point of soybean protein is around pH 4.5. As described above, the hydrolysis at around the isoelectric point of the protein is carried out under conditions of pH considerably lower than the isoelectric point of the protein, for example, under the strong acidity of soybean protein containing soybean as described above at pH 2 or less. When hydrolysis is performed, the plant fiber is decomposed too much,
In addition, the protein is also decomposed and eluted together with the plant fiber.On the other hand, when the water-insoluble plant fiber containing the protein is hydrolyzed at a neutral or alkaline pH substantially higher than the isoelectric point of the protein, the protein is degraded. This is because it is solubilized and eluted together with the plant fiber. The details of this reaction are described in JP-A-4-325008 and JP-A-3-25058.
No. 2,236,759.

The hydrolysis reaction product can be filtered or centrifuged to separate and remove solids such as undecomposed cellulose from the aqueous solution containing water-soluble hemicellulose to obtain an aqueous solution of water-soluble hemicellulose.

This hemicellulose aqueous solution contains a polysaccharide comprising galactose, arabinose, galacturonic acid, xylose, fucose, glucose, rhamnose and the like, the main component of which is a polysaccharide comprising galactose, arabinose and galacturonic acid. It is. In addition,
The details of the results of component analysis of the water-soluble hemicellulose obtained by hydrolysis are described in the above-mentioned JP-A-4-25058. By concentrating and drying this hemicellulose aqueous solution, solid water-soluble hemicellulose is obtained.

[0009] The powder granulation method of the present invention is characterized in that a hemicellulose aqueous solution is added to fine fluid droplets in a powder fluidized bed formed by fluidizing at least a part of the powder by an ascending gas flow passing through a gas dispersion plate. The method includes a granulation step of spraying as particles and causing a plurality of powder particles to adhere to each other in the presence of the fine droplet particles to form a granulated product.

FIG. 1 shows a fluidized bed granulator 1 used in the present invention.
FIG. 3 shows a schematic diagram for an example. In FIG. 1, 1 is a fluidized-bed granulator, 2 is a gas dispersion plate, 3 is a gas introduction pipe, 4 is a gas discharge pipe, 5 is a spray liquid introduction pipe made of a hemicellulose aqueous solution, 6 is a spray liquid spray nozzle, and 7 is filter,
8 denotes a heat exchanger, 9 denotes a bag filter, and F denotes a powder fluidized bed. In order to perform the powder granulation of the present invention using the apparatus of FIG. 1, after filling the powder into the apparatus 1, a fluidizing gas is introduced through a gas introduction pipe 3, and a filter 7 and a heat exchanger 8 are used. After flowing through, the gas is blown up as an ascending current through the gas dispersion plate 2 to fluidize the powder on the gas dispersion plate and form a powder fluidized bed F. The gas passing through the powder fluidized bed F is discharged through the gas discharge pipe 4 after flowing through the bag filter 9. Air is usually used as the fluidizing gas, but other gases may be used. The temperature of the fluidizing gas supplied to the powder fluidized bed F is 40 to 100 ° C, preferably 50 to 90 ° C. The temperature of the fluidizing gas is controlled by the heat exchanger 8. With respect to the powder fluidized bed F formed as described above, via the spray nozzle 6,
The spray liquid supplied through the pipe 5 is sprayed. As a result, the fluidized powder is gradually granulated, and a plurality of fluidized powder particles are formed into granules in which the fluidized powder particles are adhered and bound by the binding action of hemicellulose. In such a granulation method, as the time elapses, the particle size of the granulated material gradually increases, and accordingly, the flow rate of the fluidizing gas is increased, and the entire granulated material is in a fluidized state. To hold. After a lapse of a predetermined time, spraying of the fluidizing spray liquid is stopped, and blowing of the fluidizing gas is continued to dry the granulated material. After drying, stop blowing fluidizing gas, take out particulate matter to the outside,
Product granules. In this case, drying of the granulated material can be performed by taking out the granulated material to the outside.

The gas dispersion plate has a large number of fine through holes on the plate surface. The diameter (diameter) of this through hole is
It is 10 to 300 μm, preferably 20 to 200 μm. The diameter (diameter) of the liquid ejection hole in the spray nozzle is 0.5 to 3 μm, preferably 1.2 to 1.8 μm.
m.

The molecular weight of the water-soluble hemicellulose used in the present invention is 10 to 500 mPa · s when the viscosity at 25 ° C. of a 10% by weight aqueous solution is used as an index.
Preferably, it has a molecular weight that gives a viscosity of 15 to 100 mPa · s. The concentration of the aqueous hemicellulose solution used in the present invention is 3 to 15% by weight, preferably 4 to 12% by weight. In the hemicellulose aqueous solution, if necessary, other binders harmless to the human body, for example, gum arabic,
An appropriate amount of a water-soluble polymer such as pullulan, starch, hydroxypropylcellulose, carboxymethylcellulose and the like can be added. In addition, surfactants, coloring agents, flavors, flavors, preservatives, saccharides, and the like can be added to the aqueous hemicellulose solution in appropriate amounts. In the spray liquid comprising the aqueous hemicellulose solution used in the present invention, the viscosity of the spray liquid is 3 to 100 mpa · s, preferably 5 to 100 mpa · s.
80 mpa · s. In this case, the viscosity of the spray liquid can be adjusted by the temperature and the hemicellulose concentration. When the viscosity of the spray liquid is out of the above range, the sprayability from the spray nozzle becomes poor, and it becomes difficult to form fine droplet particles of the spray liquid having good granulation properties. In this case, the obtained granules also have a broad particle size distribution.

In the present invention, the flow velocity of the gas blown upward through the gas dispersion plate is 0.3 to 3 m / sec, preferably 0.5 to 2 m / sec as a gas linear velocity. As the gas linear velocity increases, the particle size of the granular material decreases, and the particle size is appropriately selected according to the target granule particle size. The amount of the spray liquid used in the present invention is a dry hemicellulose conversion amount,
0.1 to 10 parts by weight per 100 parts by weight, preferably 0.1 to 10 parts by weight.
It is 2 to 5 parts by weight. When the amount of use increases, the particle size of the granulated product increases, and it is appropriately selected according to the target particle size of the granulated product. The supply rate of the spray liquid is 0.03 to 1 part by weight, preferably 0.05 to 1 part by weight, based on the supply rate of dry hemicellulose per 100 parts by weight of powder per minute.
0.5 parts by weight. When the supply rate of the spray liquid exceeds the above-mentioned range, the particle size distribution of the obtained granules becomes a floating one. On the other hand, when the supply rate of the spray liquid becomes smaller than the above-mentioned range, it takes time to granulate the powder.

In the apparatus shown in FIG. 1, it is preferable to use a plurality of spray nozzles, and the spray nozzles are also arranged at a plurality of positions such as an upper portion, an intermediate portion, and a lower portion in the powder fluidized bed. Can be. As the spray nozzle, a conventional liquid spray nozzle is used. In the present invention, a spray nozzle having a two-fluid nozzle structure is preferably used. The average particle diameter (diameter) of the fine droplet particles of the spray liquid ejected from the spray nozzle is 5 to 200 μm, preferably 10 to 100 μm. When the average particle size exceeds the above range, the particle size distribution of the obtained granules becomes broader, while when the average particle size is smaller than the above range, the ratio of scattering upward from the powder fluidized bed together with the fluidizing gas is increased. And the granulation efficiency decreases.

Further, in the apparatus shown in FIG.
May be a rotatable one, for example, a rotary disk. When such a rotatable gas dispersion plate is used, the flow rate of the fluidizing gas is adjusted so that a part of the granulated material is present on the dispersion plate, and the plate surface is rotated by rotating the gas. By rolling the above granulated material, a granulated material having a spherical shape or a shape close to a spherical shape can be obtained. The rotation speed in this case is 30 to 500 m / min, preferably 5 to 500 m / min.
The speed is such that 0 to 300 m / min is obtained.

The granulated product obtained according to the present invention has an average particle size of 100 to 1500 μm, preferably 150 μm.
６００600 μm, its particle size distribution is sharp, and it is excellent in handleability, meterability and the like. The granulated product of the present invention, when its average particle size is M,
The content of particulate matter having a particle size range of 0.7M to 1.3M is 75% by weight or more, preferably 80% by weight or more.

According to the method of the present invention, since a water-soluble hemicellulose derived from a natural product is used as a binder for granulation, the granules obtained are highly safe and can be ingested into the human body. No harm. Further, in the present invention, the powder is granulated by spraying a spray liquid comprising a hemicellulose aqueous solution onto a powder fluidized bed formed by fluidizing the powder, and the viscosity of the spray liquid is 3 to 100m
Pa · s, and the spray liquid is sprayed smoothly and finely from the spray nozzle into fine droplets with good particle size uniformity and adhesion. You can get things. In addition, the granulated product of the present invention is excellent in mechanical strength.

[0018]

Next, the present invention will be described in more detail with reference to Examples. The viscosity of the spray liquid shown below was measured by a B-type clay meter.

Example 1 Lactose 7: Corn starch 3 (weight ratio) mixed powder 3 kg
Into a fluidized bed granulator (flow coater FLO-5, manufactured by Freund Corporation), and air is supplied at an air supply temperature of 30 ° C. to form a powder fluidized bed. Water-soluble hemicellulose (Hemirose, manufactured by Fuji Oil Co., Ltd.)
(The viscosity at 20 ° C. of a 10 wt% aqueous solution is 134 mPa ·
7 wt% aqueous solution (viscosity at 30 ° C .: 4)
0.5 mpa · s) as a spray liquid,
Spraying was performed at a temperature of 0 ° C. at a rate of 80 ml / min, and the mixture was granulated for 37 minutes. The amount of hemicellulose added was 3.0 wt% with respect to the mixed powder. The average particle size (diameter) of the obtained granules is about 150 μm, fine powder of less than 100 μm is 17.1 wt%, and coarse particles of 500 μm or more are 0.5 wt%.
wt%, and the mechanical strength (compressive strength) and the fluidity were also good. In this granulated product, the 0.7M
The content of the particulate matter in the range of (M is an average particle size) to 1.3 M (105 to 195 μm) was 90 wt% or more.

Comparative Example 1 The same hemicellulose powder as 3.0 wt% was added to 5 kg of the same mixed powder as in Example 1, and a high speed mixer FS / GS / 25J type (manufactured by Fukae Industry Co., Ltd., stirring granulation) 850 g of water was added dropwise little by little.
The mixture was stirred and granulated for minutes. The average particle size of the obtained granules is about 1
30 μm, and 25.0 wt.
%, The coarse particles of 500 μm or more were 6.3 wt%, and the particle size distribution was wider than that of the fluidized bed granulation, and both coarse particles and fine powder were large.

Example 2 Hemicellulose (manufactured by Fuji Oil Co., Ltd.,
S) (viscosity at 20 ° C. of a 10 wt% aqueous solution is 48.2 m)
The experiment was carried out in the same manner as in Example 1 except that a 7 wt% aqueous solution (of Pa · s) (viscosity at 30 ° C .: 17.2 mPa · s) was used.The average particle diameter of the obtained granules was about 15
0 μm, and fine powder of 100 μm or less is 15.3 wt.
%, Coarse particles of 500 μm or more were 0.2 wt%. Further, in this granulated product, the content of the granulated product having a particle size in the range of 0.7 M to 1.3 M was 90 wt% or more.

Comparative Example 2 An experiment was performed in the same manner as in Comparative Example 1 except that the hemicellulose shown in Example 2 was used. The average particle size of the obtained granules was about 150 μm, which was almost the same as that of Example 2, but
Fine powder having a size of 00 μm or less was 39.2 wt%, and coarse particles having a size of 500 μm or more were 12.2 wt%.

Example 3 An experiment was conducted in the same manner as in Example 1 except that 3 kg of lactose was used. The average particle size of the obtained granules is about 250 μm and 1
Fine powder having a size of 00 μm or less was 3.2 wt%, and coarse particles having a size of 500 μm or more were 3.8 wt%. Further, in this granulated material, the content of the granulated material having a particle size range of 0.7 M to 1.3 M was 90 wt% or more.

Comparative Example 3 An experiment was performed in the same manner as in Comparative Example 1 except that 5 kg of lactose was used. The average particle diameter of the obtained granulated product was about 250 μm, which was almost the same as that of Example 3. However, fine powder of 100 μm or less was as large as 9.3 wt%, and coarse particles of 500 μm was as large as 12.7 wt%. Was.

Example 4 An experiment was conducted in the same manner as in Example 2 except that 3 kg of lactose was used. The average particle size of the obtained granules is about 360 μm
The fine powder of 100 μm or less is 2.0 wt%, 500 μm
The above coarse particles were 2.3% by weight. Further, in this granulated product, the content of the granulated product having a particle size in the range of 0.7 M to 1.3 M was 90 wt% or more.

Comparative Example 4 An experiment was conducted in the same manner as in Comparative Example 2 except that 5 kg of lactose was used.
The average particle size of the obtained granules is about 350 μm,
Fine powder having a particle size of μm or less was as large as 10.3 wt%, and coarse particles having a particle size of 500 μm or more were as large as 11.1 wt%.

Example 5 Lactose (70% by weight) and microcrystalline cellulose (Avicel FD-1)
01) Using 3 kg of a mixed powder consisting of 30 wt%, the amount of hemicellulose added was 3.5 wt%, and the spray rate was 120
The experiment was carried out in the same manner as in Example 1 except that the granulation time was set to 15 min / ml. The average particle size of the obtained granules is about 250 μm
The fine powder of 100 μm or less is 1.0 wt%,
The amount of coarse particles having a size of μm or more was 5.9% by weight. Further, in this granulated product, the content of the granulated product having a particle size in the range of 0.7 M to 1.3 M was 90 wt% or more.

Comparative Example 5 An experiment was carried out in the same manner as in Example 5 except that a 7 wt% aqueous solution of gum arabic was used instead of the hemicellulose aqueous solution. However, the spray speed in this case was 80 ml / min, and the granulation time was 30 minutes. The average particle size of the obtained granules is about 120 μm, and fine powder of less than 100 μm is 2 μm.
7.2 wt%, coarse particles of 500 μm or more were 3.7 wt%. That is, in this case, the granulation effect was poor, and the powder was not favorable in handling such as powdering.

[0029]

According to the present invention, a specific combination of a binder for granulation and a granulation method is used, and specific granulation conditions are employed. The powder can be granulated efficiently and with high safety. Moreover, the granulated product obtained by the present invention has a sharp particle size distribution, good mechanical strength, and excellent handling properties and weighing properties.

[Brief description of the drawings]

FIG. 1 shows a schematic view of a granulation apparatus used for carrying out the method of the present invention.

[Explanation of symbols]

 DESCRIPTION OF SYMBOLS 1 Fluidized bed granulator 2 Gas dispersion plate 3 Gas introduction pipe 4 Gas discharge pipe 5 Spray liquid introduction pipe 6 Spray liquid spray nozzle 7 Filter 8 Heat exchanger 9 Bag filter F Powder fluid bed

Continued on the front page (72) Inventor Taro Takahashi 4-3 Kinudai, Yawahara-mura, Tsukuba-gun, Ibaraki Prefecture Inside Tsukuba Research & Development Center, Fuji Oil Co., Ltd. (72) Inventor Masaki Ogawa 2-chome Takadanobaba, Shinjuku-ku, Tokyo No. 2 Inside Freund Corporation (72) Inventor Takehiko Ito 2-14-2 Takadanobaba, Shinjuku-ku, Tokyo Inside Freund Corporation

Claims (4)

[Claims] 1. A method for granulating a powder of a substance to be taken into the body of an animal into a particulate having an average particle diameter of 100 to 1500 μm, wherein at least a part of the powder is raised through a gas dispersion plate. Spray liquid consisting of an aqueous solution of hemicellulose is sprayed as fine droplet particles through a spray nozzle onto a powder fluidized bed formed by fluidizing with a plurality of powders in the presence of the fine droplet particles of the spray liquid. A granulation step of adhering and bonding particles to each other to form granules, wherein the spray liquid viscosity is in the range of 3 to 100 mpa · s, and fine droplet particles of the spray liquid formed by spraying from the spray nozzle The particle size is in the range of 10 to 200 μm, and the content of the granular material in the particle size range of 0.7 M to 1.3 M (where M is the average particle size of the granulated product) in the obtained granulated product is 75% by weight or more It said method characterized by. 2. The method according to claim 1, wherein a rotatable dispersing plate is used, and the dispersing plate is rotated so as to obtain a peripheral speed of 30 to 500 m / min, and the granulated material on the dispersing plate is rolled. the method of. 3. The method according to claim 1, wherein the hemicellulose is soybean-derived hemicellulose. 4. A granulated product obtained by the method according to claim 1.