JPS6342728A - Method and apparatus for treating particulate matter - Google Patents

Abstract

PURPOSE:To easily capsulate by pressing a material to be treated against the inner surface of a casing by a centrifugal force owing to a high speed rotation to form a powder layer, and giving this powder layer compression, friction, scraping, dispersion and agitation. CONSTITUTION:A supporting body 8b and friction piece 9a are provided in a rotary shaft 8a, and a passage 27 for streaming coolant is provided in a scraping piece 9b and connected through a rotary joint 24 to a coolant storage tank 26 of the outside. The friction piece 9a and the scraping piece 9b are constructed to be rotated coaxially with a casing 4 in the same direction at a slower speed, and they give a specific compression force and friction force to the powder layer. Moreover, as necessary, the rotation of the friction piece 9a and the scraping piece 9b can be stopped to increase the relative velocity which results in increasing the agitating force.

Description

DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention relates to a powder processing method and apparatus for surface modification of powder such as mixing, granulation, spheroidization, coating, and encapsulation of powder and granules.

[Prior art]

An example of an apparatus for mixing, granulating, and drying powder and granules is disclosed in Japanese Patent Publication No. 59-48216.

In addition, for example, Tokko Kokko Sho 61-
There is a publication No. 8785. As described above, in recent years, in the pharmaceutical and food fields and in the production of new materials such as ceramics, it has become more convenient to perform the above-mentioned operations with one machine in view of the risk of foreign matter contamination and contamination.

However, there is no device, including the above-mentioned invention, that fully satisfies the mixing of finer parts of powder and granules, the spheroidization of particle units, and the coating and encapsulation of particle surfaces. Ta. Individual processing is performed using the following methods. In other words, fine mixing is carried out by using a crushing means such as a screen mill or ball mill for the premixed product, and granulation is carried out by using a scraping piece inside the rotating casing to transfer the powder on the inner peripheral surface. There is a granulator that was used. In addition, heating and melting means are used only for pelletized materials that have a low melting point and are relatively close to spherical. Furthermore, for coating powder particles, there are devices capable of attaching fine particles to the surface of powder particles.

[Problems to be Solved by the Invention] Problems with conventional means and devices for mixing fine parts, fine granulation, spheroidization, coating on surfaces, encapsulation, etc. are as follows. That is,
Fine mixing uses a pulverizing means for the mixing method, which improves the pulverizing effect on the material to be processed, but the dispersion of aggregates in the fine parts is poor, resulting in excessive pulverization of only one material, or the specific gravity of the other material. Due to the difference, even if they are mixed once, they tend to separate, making it difficult to achieve stable, uniform, and highly accurate mixing.

Furthermore, in granulation, it is difficult to use it for products with a size of 50 microns or less, and the granulation state also has a weak binding force.

By spheronizing, it has not been possible to obtain a satisfactorily spherical product for materials that are generally whisker-like or irregularly shaped.

Regarding coating on particle surfaces, it was not possible to create a product by kneading and coating the surface of fine particles with fine particles, or by injecting and coating the surface of fine particles with a colloidal substance.

Furthermore, it has not been possible to obtain fine granules by encapsulating a low-temperature vaporized substance in a capsule, such as encapsulating a fragrance using cyclodextrin, and combining it with fine powder such as pigment or resin.

The present invention solves the above-mentioned problems in processing powder and granular materials, and provides an apparatus that can perform these processes in one device.

[Means to solve the problem]

This first invention rotates a freely rotatable casing at high speed and presses the material to be treated inside against the inner circumferential surface of the casing by centrifugal force to form a powder layer, and then The purpose is to perform mixing, granulation, spheroidization, coating, encapsulation, etc. by pressing rotatably provided friction pieces and scraping pieces to apply compression and friction, and dispersion and stirring by scraping. .

Further, the second invention is a device for carrying out the first invention, in which a friction piece and a scraping piece are sequentially provided in the casing along the inner circumferential surface in the rotational direction so as to be relatively rotatable. This is because the gaps between the working surfaces of the friction pieces and the scraping pieces and the inner circumferential surface of the casing are configured so that, in the direction of rotation of the casing, the clearances for the friction pieces are narrower towards the rotational direction, while for the scraping pieces they are wider. , its functions and effects are as follows.

[Effect]

When the casing is rotated at high speed, the material to be treated is pressed against the inner circumferential surface of the casing by centrifugal force.A friction piece is constructed so that the gap between the powder layer and the inner circumferential surface decreases in the direction of rotation. The following mixing, granulation, spheroidization, coating and This allows for good encapsulation, etc.

First, regarding mixing, the multiple types of powder introduced into the casing are moderately dispersed along the inner circumferential surface, or the powder layer formed in a state where they are separated from each other is rubbed by pressing the powder layer from the surface with a friction piece. This causes partial dispersion and pushing of the powder particles into the inner layer by friction with the contact surface, and then overall stirring is performed by the scraping piece. That is, as a function of the friction pieces, the above-mentioned partial dispersion is caused by the action of loosening secondary agglomeration and tertiary aggregation on the surface of the powder layer due to friction, and the activated powder particles are similarly activated. There are two actions: adhering to other particles and compressing them, and mixing proceeds as these actions are repeated, and the next step is the overall stirring and dispersion action by scraping pieces. This is to promote mixing.

Next, regarding granulation, in addition to the above-mentioned mixing operation, water, oil,
Alternatively, by adding a small amount of one of the low melting point substances by adding a heating means if necessary, the powder starts to aggregate and becomes granulated through stirring and transfer within the casing. Note that the particle size of the granulated product becomes larger as the rotation of the casing becomes slower, and the particle size of the granulated product grows and becomes spherical as the residence time increases.

Regarding spheroidization, the spheroidization referred to here is different from the spheroidization of aggregates due to granulation described above, and is the process of making a single particle into a spherical shape. When an irregularly shaped synthetic resin or the like is compressed and rubbed by a friction piece, the frictional heat generated causes it to soften and become spherical.

For Sarani coating, when the core material is combined and put into the casing, the surface of the core material particles is activated by local friction caused by the friction pieces, and the surface of the core material particles is compressed and rubbed by the friction pieces, forming aggregates. The ultrafine coating material particles, which are dispersed and surface-activated, strongly adhere to the surface and form a coating using mechanochemical action. In addition, when the core material is a polymeric organic material, the surface of the core material particles softens and begins to mix with the coating material particles, and as time passes, the coating material particles progress into the interior of the core material particles, causing the core material particles to soften. The material particles and the coating material particles can also be integrated to create new particles with properties completely different from those of the core material particles and the coating material particles.

Encapsulation can be easily achieved by adding a colloidal substance as a capsule agent and a binder, coating the particle surface, and simultaneously drying the core substance while granulating it.

In the case of low melting point substances, they are melted by frictional heat and heating means and then cooled and encapsulated into cells while being coated on the particle surface.

In other words, the casing and friction piece are heated while the core material is compressed and dispersed in the casing, and the capsule liquid is injected while maintaining a constant temperature, and when the volatile content of the capsule liquid has completely evaporated. The heating is stopped and the product is cooled to obtain an encapsulated product.

[Effects of the Invention] As a result of the above, firstly, it has become possible to mix with high precision over minute parts. This eliminates the risk of separation after mixing, and also enables conventional mixing of grains to be performed well, resulting in a product with strong cohesive strength.

In spheronization, it is now possible to spheroidize whisker-like or irregularly shaped objects.

Regarding coating, it has become possible to coat the surface of powder particles by kneading them with fine particles. For example, it has become possible to knead and coat the surface with titanium oxide, iron oxide, pigments, and their functional inorganic/organic compounds with particle sizes of 1 to 50 microns. In addition, a colloidal substance can be injected and coated onto the surface of fine particles, and a dried product can be obtained in that state.

Regarding encapsulation, encapsulation can be carried out by adding an encapsulating agent and a colloidal substance as a binder, or an encapsulating material such as a low melting point substance, and drying or cooling. For example, liquid nitrogen is used to encapsulate low-temperature vaporized substances in capsule materials, such as encapsulating fragrances in cyclodextrin, and to combine them with fine powder particles such as pigments and resins. It became possible to obtain a finely granulated product by mixing the fine parts.

〔Example〕

Next, the present invention will be explained in detail with reference to FIGS. 1 and 2.

A bottomed cylindrical casing (4) forming a processing chamber (3) is concentrically attached to the upper end of a vertical rotating shaft (2) attached to a base (1), and an electric motor (5a) and A drive device (5) consisting of a transmission (5b) etc. is interlocked with the lower end of the rotating shaft (2), and the material to be treated inside the casing (4) is pressed against the inner circumferential surface (4a) of the casing by centrifugal force. The casing (4) is configured to be driven and rotated such that the casing (4) is rotated, and the rotational speed of the casing (4) is adjustable so as to obtain an appropriate centrifugal force depending on the properties of the material to be treated.

The casing (4) is surrounded by a cover (7), and a fan (12) is connected to the lower part of the casing (4) to suck outside air through an intake port (13) formed in the cover (7).
The structure is such that the casing (4) is cooled by the suctioned outside air, and the suctioned outside air is introduced as a gas for transporting the processed material into the transporting channel (10) connected to the cover (7). In addition, in order to transfer the processed material from the processing chamber (3) to the cover (7) side, the upper end of the casing (4) is provided with an overflow exhaust port (11) for the processed material with an opening in the center.
It is formed. A weir (21) is provided to the discharge port (11) to regulate the delivery of the processed material.

Note that the conveyance channel (10) is closed and the fan (12)
Instead, batch operation of this device is possible using a cooling and heating means such as a jacket, which will be described later.In this case, the processed material can be taken out by connecting it to an external suction device inside the processing chamber (3) after the operation is stopped. A tube is inserted and suction is applied.

Inside the casing (4), a rotating shaft (8a) that is the same as the rotating shaft (2) is fixed to the upper end, and a conical portion (
8C) is provided.

A gauging inner peripheral surface (4a) is provided at the tip of the support (8b).
) to compress, rub, scrape, and disperse and stir the material to be treated. Friction piece (9a) and scraping piece (9b)
and gauging (4) are arranged in the processing chamber (3) in order with appropriate spacing with respect to the rotational direction. Friction piece (9a
) has a gap with the casing (4).
) has an inclined surface formed so that it becomes narrower toward the direction of rotation, and conversely, the scraping piece (9b) has a wedge shape so that the gap becomes wider toward the direction of rotation, and its working surface gradually becomes wider. It is formed into a shape or a comb-like shape. Note that the rotation axis (
8a) is provided with a passage (27) for allowing a heating and cooling medium to flow into the support (8b), the friction piece (9a), and the scraping piece (9b), and a rotary joint (24). and is connected to an external medium storage tank (26). Further, the rotating shaft (8a) is attached in conjunction with the drive device (5), and has a certain rotational difference with the casing (4).
Alternatively, the friction piece (9a) and the scraping piece (9b) are set to rotate relative to each other with a constant speed difference. In other words, by configuring the friction piece (9) and the scraping piece (9b) to be driven and rotated in the same direction around the coaxial core with respect to the gauging (4) and at a slightly slower speed, the powder layer is kept constant. The compressive force and frictional force are applied. Incidentally, the friction piece (9a) and the scraping piece (9b) can be stopped to rotate if necessary, and the relative speed can be increased to increase the stirring force. The friction piece (9a) and the scraping piece (9b) have different shapes, materials,
The number of installations and others can be changed as appropriate.

In addition to forming a path (6) in the center of the cover (7) for supplying the material to be treated downward toward the conical portion (8C) of the support (8b), a pipe (14) is attached thereto. At the top, water is poured toward the inner peripheral surface (4a) of the casing.
A nozzle (22) for supplying oil, etc., and a suction pipe (23) for suctioning and discharging the treated material accumulated in the casing (4).
It is attached.

Further, a jacket (25) is provided around the cover (7) to allow a medium such as gas or liquid for heating or cooling to pass therethrough.

Furthermore, as ancillary equipment when this device is operated continuously, a collector (15) and an exhaust fan (16) are connected to the flow path (lO) in that order, and the exhaust port of the collector (15) is connected to the flow path (lO). is connected to the supply route (6) by a row feeder (17),
It is configured so that some parts that are insufficiently processed can be processed again.

A blower (13) that supplies an appropriate amount of heated and cooled air or inert gas as necessary, a feeder (19) for supplying the material to be processed, and a feeder (19) that supplies the material processed in another process ( 20) is connected to the supply path (6), so that a supply form can be adopted depending on the condition of the material to be treated.

The gas sent to the cover (7) can be appropriately selected depending on the material of the material to be treated, and an appropriate air supply means depending on the type of gas, such as an electric blower or a pressurized gas cylinder, can be used. . These are collectively referred to as an air supply device (12).

Ancillary equipment as a processing apparatus, such as equipment for supplying processed materials to the processing chamber (3) and equipment for recovering processed materials, can be freely changed, added, or omitted.

[Another example]

As another embodiment, the device may be in a horizontal arrangement with a horizontal or inclined axis of rotation, and the friction piece of the invention may be a cylindrical roller, which is placed around the inner periphery of the casing (4a). By relative rotation, the same effect as that of the friction piece (9a) can be obtained.

In addition to supplying heated or cooled air or inert gas into the processing chamber (3), a refrigerant such as liquid nitrogen is directly introduced into the casing (4) for the purpose of cooling the processing chamber (3). Good too.

In addition to pigment glazes, toners, printing/transfer materials, food, feed, fertilizers, pharmaceuticals, industrial chemicals, ultraviolet sterilization, sterilizing materials, main conditioners, disk materials, liquid crystal materials, etc., it can also be used as a standard powder.

Experimental examples are described below.

(Experiment example 1) Titanium oxide with a particle size of 0.01 to 0.2 μ and an average particle size of 0°0
A mixture of ferric oxides of 0.05μ and 1% to 99%, respectively, is finely mixed by complete dispersion in water.

(Experiment Example 2) Ultrafine mica powder, titanium oxide, alumina, silicon oxide, and colloidal silica are mixed and deposited into a spherical shape to produce ultrafine mica powder.
Average particle size 0.6μ 40% titanium oxide 〃0.
1μ 15% alumina 〃0.1μ 5%
Silicon oxide // 0.05μ 20% colloidal silica // 0.015μ
20% (solid content) concentration 20% Temperature 180°C to 250°C Product 1 to 100μ spherical granules (Figure 3) (Experiment Example 3) Spongy and whisker-like tetrafluoroethylene resin was spheroidized into spherical and elliptical shapes. The raw material is anisotropic, spongy, and whisker-like with a size of 20 to 100 μ (Figure 4), and after 5 minutes it becomes 10
~30μ spherical shape and elliptical shape (Figure 5), and after 40 minutes 30~60μ (Experimental Example 4) Particle size 0.1~0.
A 2 μm titanium oxide powder was coated using static electricity and thermal softening. (Figure 7) Applications include cosmetics.

(Experiment Example 5) Average particle size of 0.015 to J3 resin sphere with average particle size of 2μ
To coat μ's titanium oxide, we first rubbed the surface of the silicone sphere to activate it, added the titanium oxide, and at the same time compressed it under heat to coat it. (Figure 8)
As a result of this coating, the hydrophobic silicone properties were changed to hydrophilic.

(Experimental Example 6) The surface of the silicone sphere coated with titanium oxide produced in the above (Experimental Example 5) was further coated with iron oxide. (Figure 9) Iron oxide uses fatty acids as a dispersant and has an average particle size of 0.
005μ.

As a result, what had become hydrophilic due to the titanium oxide coating returned to hydrophobic properties, increasing oil absorption. Applications include cosmetics, mold release agents, and pigments.

(Experimental Example 7) Titanium oxide with an average particle size of 0.015 μm was kneaded and coated on the surface of methyl methacrylate spheres with an average particle size of 6.7 μm. (Figure 10) This is because when the temperature of the casing exceeds the glass transition point of methyl methacrylate and the surface temperature of methyl methacrylate reaches nearly 200°C due to friction, the kneading effect with titanium oxide occurs on the surface. This begins to occur, and as the operation continues, titanium oxide diffuses into the methyl methacrylate. As a result, the composite material thus produced is a highly dispersible spherical particle with a negative electrostatic charge and zero angle of repose.

It can be used in cosmetics, toners, pigment bases, paints, etc., as well as as a standard powder.

[Brief explanation of the drawing]

The explanatory diagram, FIG. 2, is a sectional view taken along the line ■-■ in FIG. FIGS. 3 to 10 are micrographs of experimental examples in this example. (3)...Processing chamber, (4)...Casing, (4a)...Casing inner peripheral surface, (5)...
... Drive device, (7) ... Cover, (9a
)... Friction piece, (9b)... Scraping piece, (10)... Channel for conveying processed material, (11)
...Overflow set outlet, (12)...
...Air supply device, (15) ...Collector, (22
)... Nozzle, (23)... Suction pipe. Applicant: Honkawa Micron Co., Ltd. Figure 5 5Fj %) B, oo (14) AI Figure 4 Figure 6 Figure 7 Figure 9 Whistle 1n 1 (3o, ooo'@) AI Procedural Amendment Document Showa 1 year II month zt Date of 1986 Patent Application No. 186642 2 Name of the invention Powder processing method and device 3 Relationship with the case by the person making the amendment (Patent applicant) Address: 2-14-5 Osaka Kataoka, Osaka-shi, Osaka 552 Name
Hosokawa Micron Co., Ltd. Representative Masu Hosokawa
Man 4, Date of the amendment order: October 8, 1985 5, Column 6 for a brief explanation of the drawings in the specification subject to amendment, Contents of the amendment 4, Brief explanation of the drawings Figures 1 and 2 are from this book. Embodiments of the invention are shown; FIG. 1 is a schematic cross-section of the main parts of the processing apparatus and an explanatory diagram of incidental equipment, and FIG. 2 is a cross-sectional view taken along the line ■--■ in FIG. In the figure, 3...processing chamber, 4...casing, 4a...casing inner peripheral surface, 5...
...Drive device, 7...Cover, 9a...
...Friction piece, 9b... Scraping piece, 10...
... Processing material conveyance channel, 11 ... Overflow set outlet, 12 ... Air supply device, 15 ...
... Collector, 22 ... Nozzle, 23 ...
...Suction pipe Figures 3 to 10 are electron micrographs of the particles of cosmetics, etc. obtained in this example, and Figure 3 shows the granulated product obtained in Experimental Example 2. 8000x electron micrograph, Figure 4 is an electron micrograph magnified 500x of the whiskers of the tetrafluoroethylene resin used in Experimental Example 3, and Figure 5 is a photograph taken 5 minutes after the start of operation in Experimental Example 3. Figure 6 is a 500x electron micrograph of the granulated product obtained after 40 minutes of operation in Experimental Example 3, and Figure 7 is a 500x electron micrograph of the granulated product obtained in Experimental Example 4. Figure 8 is an electron micrograph of the cosmetic particles coated in Experimental Example 5 at a magnification of 80,000 times, and Figure 9 is an electron micrograph of the cosmetic particles coated in Experimental Example 6 at a magnification of 80,000 times. FIG. 10 is an electron micrograph of the cosmetic particles obtained in Experimental Example 7, magnified by 500 times. Procedural amendment 1962 Hirotsuki 2? Day 1, Indication of the case 1986 Patent Application No. 186642 2, Name of the invention Powder processing method and apparatus 3, Person making the amendment Relationship with the case (patent applicant) Address: Osaka Kataoka, Osaka City, 552 2-chome 14-5 Name
Hosokawa Micron Co., Ltd. 4. Date of amendment order Vol. 6. Contents of amendment (1) Page 7 of the specification, lines 7 to 11, ``Next, regarding granulation... ."teeth,
The following corrections are made. [Next, for granulation, in addition to the above-mentioned mixing operation, a small amount of water, oil or fat, or a low melting point substance is added, and a heating means is added as necessary. As a result, the mixing operation uniformly mixes the powder particles with liquids such as water, oil, and fats, and low-melting substances, and the powder particles begin to agglomerate sequentially and become granulated by stirring and transfer within the casing. be converted into ” (2) On page 9 of the specification, lines 11 to 12, “Also, conventionally...
・・・・・・It has become possible. ” is corrected as follows. "Also, it has become possible to mix things that could not be mixed in the past, such as powders with large differences in specific gravity, with high precision, or to add a small amount of liquid and disperse it uniformly into the powder." 3) Page 12 of the statement, lines 3 to 6
The line "It is possible..." should be corrected as follows. [In addition, by lowering this weir (21), the discharge port (1
1) can be closed and can be switched to batch operation without the need for a separate lid. Therefore, the conveying channel (10) is closed, the fan (12) is removed, and instead, batch operation of the apparatus is enabled by cooling and heating means such as a jacket, which will be described later. (4) "1 to 99%" on page 16, line 14 of the statement will be corrected to "1 to 99." (5) On page 19 of the specification, lines 3, 6, 7, and 10, “
``Methyl methacrylate'' has been corrected to ``Polymethyl methacrylate.''

Claims (4)

[Claims] (1) A rotatably installed casing is rotated at high speed to press the material to be treated against the inner peripheral surface of the casing by centrifugal force to form a powder layer, and the powder layer is subjected to compression, friction, and scraping. Dispersion, stirring, addition of liquid, heating,
A method for processing powder and granular material, characterized in that mixing, granulation, spheroidization, coating, and encapsulation are performed by adding cooling means. (2) A drive device is connected to the freely rotatable casing, which rotates the material inside the casing at high speed so as to press the material to be processed against the inner circumferential surface of the casing by centrifugal force. The casing and the scraping piece are provided so as to be relatively rotatable in order in the direction of rotation, and the casing,
A powder processing device characterized in that a heating and cooling mechanism is connected to a friction piece and a scraping piece. (3) The powder/granular material processing apparatus according to claim (2), wherein the friction piece is formed so that a gap with the inner circumferential surface of the casing becomes narrower toward the rotational direction of the casing. (4) The scraping piece has a gap with the inner circumferential surface of the casing that becomes wider toward the rotational direction of the casing, and its working surface has a wedge-like or comb-like shape that becomes wider toward the rotational direction of the casing. Said claim No. (
2) The powder and granular material processing apparatus described in section 2).