WO2013032002A1

WO2013032002A1 - Surface modification device for solid particles and surface modification method for solid particles

Info

Publication number: WO2013032002A1
Application number: PCT/JP2012/072289
Authority: WO
Inventors: 自起奈良
Original assignee: 株式会社奈良機械製作所
Priority date: 2011-08-31
Filing date: 2012-08-28
Publication date: 2013-03-07
Also published as: JP5648124B2; JPWO2013032002A1

Abstract

The purpose of the present invention is to provide a device capable of efficiently drying or cooling in accordance with the type of liquid, and capable of satisfactorily and with good productivity surface-modifying solid particles. In order to achieve this purpose, this surface modification device for solid particles has: a rotating disc having shock pins arranged around the periphery thereof, arranged inside an impact chamber; a collision ring arranged along the outermost peripheral race surface of the shock pins, separated a set space from same; a circulation circuit pipe (20) for guiding and circulating, together with the processing powder, airflow that is generated by the rotation of the shock pins, said circulation circuit pipe disposed such that one opening of same opens to part the collision ring and the other opening opens to the front cover in the vicinity of the center of the rotating disc; a spray nozzle (22a) that supplies liquid to either the front cover, the collision ring, or the circulation circuit pipe; a supply port (23) that supplies a heating medium, a cooling medium, or a drying medium to an appropriate location in the circulation circuit pipe; and a discharge port (24) that discharges excessive circulation air.

Description

Solid particle surface modification apparatus and solid particle surface modification method

The present invention relates to a surface modification device for solid particles and a surface modification method for solid particles. More specifically, on the surface of the solid particles, a dispersion in which other fine solid particles are dispersed in a liquid, a solution in which a solute of a solid component is dissolved in a liquid, a melt of a solid component, etc. The liquid material) is applied to the solid particles, impact force is applied to the solid particles, and the liquid material is dried or cooled to embed or fix the fine solid particles on the surface of the solid particles, or to the surface of the solid particles. The present invention relates to an apparatus and a method for immobilizing a solid component in a film shape and modifying the surface of solid particles.

Conventionally, various surfaces of powder for the purpose of preventing sticking, preventing discoloration / discoloration, improving dispersibility, improving fluidity, improving catalytic effect, controlling digestion / absorption, improving magnetic properties, improving weather resistance, etc. Modifications have been made.
In this, other solid particles smaller than this solid particle (hereinafter also referred to as “child particle”) are embedded or fixed on the surface of the core solid particle (hereinafter also referred to as “mother particle”). Then, a method of obtaining a functional composite powder material whose surface of the solid particles has been modified (hereinafter sometimes referred to as “an immobilization method”), a child particle is immobilized on the surface of the mother particle in the form of a solid A method of obtaining a functional composite powder material having a modified particle surface (the “film-forming treatment method”) and a method of spheroidizing amorphous solid particles such as metals, resins, and inorganic substances (same as above) , “Spheronization processing method”). As a method for carrying out these, for example, Japanese Patent Publication No. 3-2009, Japanese Patent Publication No. 3-76177, Japanese Patent Publication No. 4-3250, Japanese Patent Publication No. 5-10971 There is a high-speed impact-in-air impact method disclosed in.
According to the high-speed air-flow impact method disclosed in these patent publications, a rotating disk having hammer-type or blade-type impact pins arranged around a casing is disposed in the casing, and along the outermost raceway surface of the impact pins. A front cover that constitutes a casing through a circulation circuit from a circulation port that opens a part of the inner wall of the collision ring for the air flow generated by the rotation of the impact pin by arranging the collision ring with a certain space. It is guided and circulated from the opening of the central part to the impact chamber (self-circulating flow), and the treated powder is repeatedly passed through the impact chamber and the circulation circuit together with the air flow, and mechanical impact by the impact pin and the impact ring Uniform powder processing is performed in a short time (several tens of seconds to several minutes) by impact-type impact action by collision.
In particular, the impact method in high-speed air current disclosed in Japanese Patent Publication No. 5-10971 discloses that the liquid material is attached to the surface of the mother particle, giving impact force to the mother particle, and drying or cooling the liquid material. Then, the child particles are embedded or fixed on the surface of the mother particles, or the solid component is fixed in the form of a film to modify the surface of the solid particles.
Here, any of the above high-speed air-flow impact methods is a complete batch processing method. In particular, in the method disclosed in Japanese Patent Publication No. 5-10971 which performs surface modification of solid particles by embedding or fixing child particles on the surface of mother particles or fixing solid components in a film shape, There is no means for supplying a medium for actively drying the liquid into the apparatus. Therefore, depending on the type of the liquid material, it takes a long time to dry the liquid material, the productivity is low, and the quality of the product obtained by the surface modification treatment may be poor.
Therefore, conventionally, there has been adopted a method in which a collision structure, a circulation circuit, and further, if necessary, the inside of a rotating disk have a jacket structure, and a heating medium is heated through the jacket. In addition, a method of heating air or an inert gas introduced into the impact chamber and the circulation circuit in advance by a known means has been adopted.
However, in the heating method using the former jacket structure, since heat exchange uses indirect heat conduction, the heating effect is limited. In the latter case, since it is a complete batch type device, only a small amount of air present in the impact chamber and the circulation circuit is replaced with preheated air or inert gas. It was insufficient.

The present invention has been made in view of the above-described problems of the background art, and the object thereof is to efficiently dry or cool the liquid according to the type of the liquid, and the solid particles have good productivity and good quality. It is an object of the present invention to provide an apparatus and method capable of performing surface modification treatment.
In order to achieve the above-mentioned object, the present invention provides the solid particle surface modifying apparatus and solid particle surface modifying method described in [1] to [9] below.
[1] In the impact chamber, a turntable with impact pins is disposed, and a collision ring is disposed along the outermost raceway surface of the impact pins and with a certain space with respect to the impact pin. A circulation circuit tube for guiding and circulating the processing powder together with the air flow generated by the rotation of the pin, one opening of the circulation circuit tube is opened in a part of the collision ring, and the other opening is formed in the rotating disk. A spray nozzle is provided to be opened in the front cover near the center, and a liquid nozzle is provided to supply the liquid material to any one of the front cover, the collision ring, or the circulation circuit tube. A solid particle surface reforming apparatus comprising a supply port for supplying a medium and an exhaust port for discharging excess circulating gas.
[2] The above-mentioned [1], wherein the supply port is provided in the circulation circuit tube, and the exhaust port is provided in the circulation circuit tube located on the downstream side of the supply port. Solid particle surface modification equipment.
[3] The surface modification device for solid particles according to [1] or [2], wherein a part of the circulation circuit tube is expanded to form an enlarged portion.
[4] The solid particle surface modification according to [3], wherein the enlarged portion of the circulation circuit tube is formed between the downstream side of the supply port and the upstream side of the exhaust port. Quality equipment.
[5] The solid particle surface reforming apparatus according to any one of [1] to [4], wherein a powder recovery apparatus is connected to the exhaust port.
[6] The spray nozzle that supplies the liquid material to the upstream end of the circulation circuit pipe is provided, and the supply port is provided in a part of the circulation circuit pipe that is located immediately downstream of the spray nozzle. Any one of [1] to [5] above, wherein the exhaust port is provided in a portion of the circulation circuit tube that is downstream and relatively close to the upstream end side. Solid particle surface modification equipment.
[7] The surface modification apparatus for solid particles according to any one of [1] to [5], wherein a spray nozzle for supplying a liquid material is provided at a downstream end of the circulation circuit tube. .
[8] Using the solid particle surface modifying apparatus according to any one of [1] to [7] above, the solid particles for surface modification are charged into the apparatus separately from the liquid, and A surface modification method for solid particles, characterized by performing surface modification.
[9] Using the solid particle surface modifying apparatus according to any one of [1] to [7], the solid particles to be surface-modified are dispersed in the liquid and the apparatus is disposed through the spray nozzle. The method for surface modification of solid particles is characterized in that the surface modification of solid particles is carried out.
According to the above-described surface modification device or surface modification method for solid particles according to the present invention, the heating medium, the cooling medium, or the drying medium is directly supplied and brought into contact with the airflow that circulates with the processing powder. In particular, a liquid containing child particles and the like can be efficiently dried or cooled. For this reason, the operation of modifying the surface of the solid particles with good productivity and goodness by embedding or fixing the fine solid particles on the surface of the solid particles or fixing the solid component on the surface of the solid particles in the form of a film. An apparatus or method that can be performed.
Further, according to the surface reforming apparatus or the surface reforming method of the solid particles according to the present invention, the exhaust gas exhaust port for exhausting excess circulating gas is provided, so that the circulating gas inside the apparatus is supplied even if a heating medium or the like is supplied. The amount can be maintained at an appropriate value. Therefore, the apparatus or method can supply an appropriate amount of heating medium or the like without adding to the apparatus.
Furthermore, when a supply port for supplying a heating medium or the like is provided in the circulation circuit tube and an exhaust port for discharging excess circulation gas is provided in the circulation circuit tube located on the downstream side of the supply port, The circulation circuit tube is the main drying or cooling unit. For this reason, drying or cooling is performed well in this portion, and the heating temperature is easily controlled. In addition, in the case of an apparatus in which a part of the circulation circuit tube is enlarged to form an enlarged part, the flow rate of the circulating gas is reduced in the enlarged part, and heat exchange with the supplied heating medium is good. It becomes the device performed in. Further, when the enlarged portion is an apparatus formed between the downstream side of the supply port and the upstream side of the exhaust port, the flow rate is not increased particularly by supplying a heating medium or the like. In addition, when the powder recovery device is connected to the exhaust port for discharging excess circulating gas, the powder in the exhaust fluid can be separated and recovered, and the exhaust can be made clean. . Furthermore, a spray nozzle for supplying a liquid material containing small particles or the like is provided at the upstream end of the circulation circuit tube, and a supply port for supplying a heating medium or the like is provided at a portion of the circulation circuit tube located immediately downstream of the spray nozzle. When the apparatus is provided with an exhaust port for discharging excess circulating gas at a portion of the circulation circuit tube located downstream of the supply port and relatively close to the upstream end side, the supplied heating medium The heat exchange between the medium such as the liquid and the liquid containing the small particles is particularly efficient, resulting in a device having higher drying or cooling processing efficiency. Moreover, when it is set as such an apparatus, it becomes an apparatus with few particles discharged | emitted with an excess circulating gas from an exhaust port. In addition, when the apparatus is provided with a spray nozzle for supplying a liquid material to the downstream end of the circulation circuit tube, the liquid material containing the child particles can be sprayed on the surface of the solid particles immediately before the impact or impact is applied. It becomes a device.

FIG. 1 is a front view showing an embodiment of a surface reforming apparatus for solid particles according to the present invention together with incidental equipment.
FIG. 2 is a side view of the apparatus shown in FIG.
FIG. 3 is an enlarged cross-sectional view of a portion along line AA in FIG.
FIG. 4 is a diagram showing an example of a circulation circuit tube, where (a) is a front view, (b) is a plan view, and (c) is a partial side view.

DESCRIPTION OF THE PREFERRED EMBODIMENTS Embodiments of a solid particle surface modifying apparatus and a solid particle surface modifying method according to the present invention will be described below in detail with reference to the accompanying drawings.
1 to 4, reference numeral 1 denotes a casing of the surface reforming apparatus, 2 denotes a front cover of the casing 1 as shown in FIG. 3, and 3 denotes a rear cover of the casing 1. Reference numeral 4 denotes a rotating disk provided in the casing 1 which rotates at a high speed, and 5 denotes a plurality of impact pins radially provided around the outer periphery of the rotating disk 4 with a predetermined interval. The impact pin 5 is generally of a hammer type or a blade type. Reference numeral 6 denotes a rotating shaft that rotatably supports the rotating disk 4. Reference numeral 7 denotes a collision ring which is provided along the outermost raceway surface of the impact pin 5 and is provided with a certain space with respect to it. The collision ring 7 is of an uneven type or a circumferential plane type having various shapes. Here, the fixed space varies depending on the size of the apparatus, but is generally preferably 0.5 to 20 mm.
Reference numeral 8 denotes an impact chamber surrounded by the front cover 2, the rear cover 3 and the collision ring 7. Reference numeral 9 denotes a processing powder discharge port provided by cutting out a part of the front cover 2. In some cases, the discharge port 9 may be provided by notching a part of the collision ring 7 or a circulation circuit tube described later. Reference numeral 10 denotes a charging port for the solid particles opening near the center of the front cover 2 (also a charging port for the liquid material into the shock chamber 8). The discharge port 9 is provided with an opening / closing valve 11, and the opening / closing valve 11 is opened / closed by an actuator 12. As shown in FIG. 1, 13 is a discharge pipe connected to the discharge port 9 via the on-off valve 11, and 14 is a product tank (bag filter) connected to the discharge pipe 13. A raw material hopper 16 is connected to the charging port 10 via a charging pipe 15. Reference numeral 17 denotes an open / close valve (ball valve) provided in the middle of the charging pipe 15.
As shown in FIG. 4, reference numeral 20 denotes a circulation circuit tube having one end connected to a circulation port 21 opening in a part of the inner wall of the collision ring 7 and the other end connected to the solid particle inlet 10. . The circulation circuit tube 20 is formed in a substantially U shape. A part of the circulation circuit tube 20 (from the upstream straight portion to the entire curved portion) is enlarged in diameter and formed in the enlarged portion 20a. The volume of the circulation circuit tube 20 is designed to be about 0.2 to 5 times the volume of the impact chamber 8. If the volume of the circulation circuit tube 20 is smaller than this, the liquid cannot be efficiently dried or cooled. On the other hand, if it is larger than this, the number of times of circulation of the processing powder such as solid particles is greatly reduced, so that the surface modification treatment takes a long time. From this point of view, the volume of the circulation circuit tube 20 is more preferably designed to be 0.5 to 3.5 times the volume of the impact chamber 8. Here, the circulation port 21 is provided in a normal direction to the collision ring 7 in the apparatus according to the illustrated embodiment. However, the circulation port 21 may be provided tangential to the collision ring 7. The ratio of the diameter expansion in a part of the circulation circuit tube 20 is preferably 1: 1.05 to 1: 2 in terms of the inner diameter ratio. In addition, in the apparatus according to the illustrated embodiment, the circulation circuit tube 20 has a volume from the connecting portion of the charging tube 15 connected to the other end to the charging port 10 in addition to the internal volume of the circulating circuit tube 20. The internal volume of the tube 15 is also included. Note that the ratio of the diameter expansion is determined based on the flow velocity of the gas circulating in the circulation circuit tube 20. That is, the velocity of the airflow in the circulation circuit tube 20 directly above the circulation port 21 through which only the airflow generated by the rotation of the impact pin 5 flows and the heating medium supplied from the supply port described later flow together. The velocity of the airflow in the circulation circuit tube 20 after the supply port is made substantially the same.
22a and 22b are liquid spray nozzles supplied to the apparatus for modifying the surface of the mother particles, which are solid particles. In the present invention, a liquid is a dispersion in which other fine solid particles used for surface modification of solid particles are dispersed in a liquid as defined above, a solution in which a solute of a solid component is dissolved in a liquid, a solid component However, the solid particles for surface modification may be contained in a dispersed state. The

spray nozzles

22a and 22b are provided at two locations, the upstream end and the downstream end of the circulation circuit tube 20, respectively. Either of these

spray nozzles

22a and 22b may be used during operation, or both may be used. The

spray nozzles

22a and 22b are connected to a liquid supply device (not shown). The

spray nozzles

22a and 22b are also supplied with compressed air for finely spraying the liquid material. Reference numeral 23 denotes a heating medium, a cooling medium or a drying medium (collectively referred to in this specification) provided in a portion of the circulation circuit tube 20 located immediately downstream of the spray nozzle 22a provided on the upstream end side. This is a supply port for supplying “circulation circuit tube 20” in some cases. Examples of the heating medium supplied from the supply port 23 include compressed air heated to a constant temperature by a heating device. Examples of the cooling medium include compressed air cooled to a constant temperature by a cooling device, and low-temperature gas obtained by vaporizing a refrigerant such as liquid nitrogen or dry ice. In addition, when no heating or cooling medium is required, compressed air dehumidified by a dehumidifying device is used as a drying medium. The supply port 23 is connected to a supply device that supplies any one of these media. The supply port 23 is provided in the circulation circuit tube 20 with respect to the flow direction of the airflow in order to quickly disperse the liquid material supplied from the spray nozzle 22a by the ejector effect in the flow of airflow in the circulation circuit tube 20. And are preferably connected at an acute angle. The

spray nozzles

22a and 22b are also preferably connected to the circulation circuit tube 20 at an acute angle with respect to the flow direction of the airflow for the same reason.
Reference numeral 24 denotes an exhaust port for discharging excess circulating gas. The exhaust port 24 is provided on the downstream side of the supply port 23 for supplying the heating medium and the like and in a portion of the circulation circuit tube 20 at a position relatively close to the upstream end side. This is because the processing powder such as solid particles circulates in the circulation circuit tube 20 along with the air flow generated by the rotation of the impact pin 5 and the heating medium supplied from the supply port 23, etc. The speed difference will be slowed down. And when the speed of solid particles etc. becomes slow, it will become easy to discharge | emit with the excess circulation gas exhausted from the exhaust port 24. FIG. Therefore, excessive circulating gas is discharged while the speed of solid particles or the like is as fast as possible. Further, in the U-shaped portion of the circulation circuit tube 20, solid particles and the like circulate along the inner surface of the tube on the outer peripheral side. Therefore, the exhaust port 24 is connected to the circulation circuit tube 20 at an acute angle with respect to the flow direction of the airflow, as shown in FIG. 4 (a), on the inner peripheral side of the U-shaped portion. This is preferable because solid particles and the like are not easily removed. The exhaust port 24 is connected to an ejector pump using compressed air through an exhaust pipe (not shown).
Even with the connection method of the exhaust port 24 as described above, the fine solid particles in the dispersion or the fine solid particles in the solution produced by spray drying may be discharged together with the excess circulating gas. Therefore, a powder recovery device (not shown) is connected in the middle of the discharge pipe. As this powder recovery device, an external filtration type bag filter is preferable. In this case, the filter may be fixed or rotating. When the filter is a fixed type, it has an outer cylinder surrounding the filter and has a backwashing mechanism, and the material of the filter is preferably, for example, polyester felt Teflon laminate (Teflon is a registered trademark). Even when the filter is a rotary type, the outer cylinder surrounds the filter, and the material of the filter is preferably a sintered metal (for example, SUS316).
Here, in the embodiment described above, the

spray nozzles

22 a and 22 b for supplying the liquid material are provided in the circulation circuit tube 20. However, the

spray nozzles

22 a and 22 b may be provided in any part of the front cover 2 and the collision ring 7 that define the impact chamber 8. Further, when the liquid material is dried by effectively using the heating medium or the like supplied from the supply port 23, the exhaust port 24 is rather the rear end of the circulation circuit tube 20 contrary to the above-described embodiment. That is, it is preferably provided in the vicinity of the connection portion with the input pipe 15. In addition, as another method for exhausting excess circulating gas from the circulation circuit tube 20, there is a method in which a part of the circulation circuit tube 20 is piped with a filter. Specifically, a plurality of holes are formed in a part of the circulation circuit tube 20, the hole part is covered with a cylindrical filter, and the filter part is surrounded by a cylinder closed at both ends. The cylinder is provided with an exhaust port 24 and connected to an ejector pump by compressed air through an exhaust pipe in the same manner as described above. In this case, the inner surface of the filter may be clogged with solid particles or fine solid particles. Therefore, it is preferable to provide a structure in which a plurality of holes for backwashing are provided on the side surface of the cylinder, and compressed air is periodically supplied from the holes to be removed. In this case, the filter material is preferably a Teflon woven fabric (Teflon is a registered trademark).
In addition, in the figure, reference numeral 40 denotes a control device for controlling the operation of the surface reforming apparatus and incidental facilities according to the present invention. The operation condition of the apparatus is set by the control apparatus 40, the operation is performed in a controlled state, and the current value, the rotation speed, the temperature, and the like during the operation are monitored.
Next, an operation method of the above apparatus will be described using an example in which the surface of the solid particles (mother particles) is subjected to surface modification treatment using a dispersion liquid in which other fine solid particles (child particles) are dispersed. However, the operation method of the apparatus is not limited to this operation method.
First, the on-off valve 11 for discharging the treated powder provided in the casing 1 is closed. Subsequently, the rotating shaft 6 is driven by a driving means (not shown), and the rotating disk 4 is moved at an appropriate peripheral speed between 5 m / sec and 160 m / sec, for example, a peripheral speed of 100 m / sec, depending on the properties of the mother particles to be processed. Rotate. At this time, an abrupt air flow is generated with the rotation of the impact pin 5 provided on the outer periphery of the rotating disk 4. Then, the circulation flow of the airflow returning to the central portion of the rotating disk 4 from the circulation port 21 opening to the impact chamber 8 through the circulation port 21 by the fan effect based on the centrifugal force of the airflow, that is, the self-circulation flow is generated in the apparatus. Formed.
Next, a medium suitable for the mother particles, for example, hot air heated to, for example, 60 ° C. by a heating device (not shown) is supplied into the circulation circuit tube 20 from the supply port 23 such as a heating medium. Then, the temperature of the entire surface reformer is increased by this hot air. The supply amount of hot air can be arbitrarily set according to the temperature of the hot air, the supply amount of the liquid, the processing time, and the like. Hot air is supplied from the supply port 23, and excess circulating gas in the same amount as the hot air is discharged from the exhaust port 24 by an ejector pump (not shown).
Next, a certain amount of solid particles, that is, mother particles, is put into the impact chamber 8 by opening the opening / closing valve 17 from the raw material hover 16. Then, the mother particles are repeatedly circulated between the circulation circuit tube 20 and the impact chamber 8 along with the self-circulating flow of the airflow. Then, after confirming that no mother particles remain in the raw material hopper 16, the on-off valve 17 is closed.
Subsequently, the dispersion liquid in which the child particles are dispersed is supplied to the spray nozzle 22a at a constant flow rate using a tube pump or the like from a container in which the child particles are placed, and compressed air is supplied to the spray nozzle 22a. Then, the dispersion liquid is sprayed into the circulation circuit tube 20. The dispersion liquid supplied from the spray nozzle 22a into the circulation circuit tube 20 adheres to the surface of the mother particles moving in the circulation circuit tube 20 along with the air flow.
Hot air is continuously supplied into the circulation circuit tube 20 from the supply port 23. For this reason, the dispersion liquid is heated and dried before the mother particles to which the dispersion has adhered return to the impact chamber 8, and only the child particles in the dispersion remain on the surface of the mother particles. The mother particles with the child particles adhering to the surface are subjected to momentary impact action by the large number of impact pins 5 of the rotating disk 4 rotating at a high speed in the impact chamber 8 and collide with the surrounding collision ring 7. Receives strong compressive action. Therefore, the child particles are firmly fixed on the surface of the mother particle. In addition, although it changes with operating conditions, the supply time of the dispersion liquid is usually several tens of seconds to several minutes.
On the other hand, the circulating gas that has become excessive due to the supply of the heating medium or the like from the supply port 23 is discharged from the exhaust port 24 provided in the circulation circuit tube 20. At this time, as in the apparatus according to the illustrated embodiment, the exhaust port 24 is provided on the downstream side of the supply port 23 for supplying a heating medium or the like and relatively close to the upstream end side. When provided, the flow velocity of the mother particles flowing along with the circulating gas is still high at this position. Therefore, it is possible to reduce the number of particles that come out of the system from the exhaust port 24 along with the discharged gas. Further, a powder recovery device is connected to the exhaust port 24. Therefore, the powder particles are captured by the powder recovery device, and clean exhaust is discharged to the atmosphere. In addition, the child particles that are not particularly attached to the surface of the mother particles are selectively discharged from the system together with the air flow from the exhaust port 24. Therefore, surplus child particles do not remain in the product, which can contribute to the stability of product quality.
Depending on the purpose of processing after the supply of the dispersion liquid is completed, the operation of the apparatus is continued for several tens of seconds to several minutes as necessary to fix the child particles, homogenize the film, make the mother particles spherical, etc. There are things to do. Further, the supply of the dispersion and the subsequent immobilization treatment can be repeated in several times. Furthermore, on the layer of the child particle fixed on the surface of the mother particle, another child particle is further fixed, or the child particle is fixed in a film shape to prepare a multilayered solid particle. You can also
After the above fixing operation is completed, the on-off valve 11 for discharging the processed powder is opened by the actuator 12, and the fixed powder is discharged. The fixed powder is discharged from the impact chamber 8 and the circulation circuit tube 20 through the discharge port 9 in a short time (several seconds) by the centrifugal force acting on itself by the rotation of the impact pin 5. The The discharged powder is captured by the product tank (bag filter) 14 through the discharge pipe 13. After discharging the fixed powder, the on-off valve 11 is closed, and the next base particle is weighed and put into the raw material popper 16. Then, the dispersion liquid containing the mother particles and the small particles is again supplied into the apparatus, and the fixed powder is produced through the same process as described above. The series of batch immobilization processing operations are controlled by the control device 40 set in advance in a time-related manner and are continuously operated in relation to the operation time of the related equipment.
As described above, the solid particle surface modification apparatus or surface modification method of the present invention directly supplies and contacts the heating medium or the like in the air stream circulating with the treated powder, so that the treated powder, in particular, The liquid containing the child particles can be efficiently dried or cooled. For this reason, the operation of modifying the surface of the solid particles with good productivity and goodness by embedding or fixing the fine solid particles on the surface of the solid particles or fixing the solid component on the surface of the solid particles in the form of a film. An apparatus or method that can be performed.
Further, according to the surface reforming apparatus or the surface reforming method of the solid particles according to the present invention, the exhaust gas exhaust port for exhausting excess circulating gas is provided, so that the circulating gas inside the apparatus is supplied even if a heating medium or the like is supplied. The amount can be maintained at an appropriate value. Therefore, the apparatus or method can supply an appropriate amount of heating medium or the like without imposing a load on the apparatus.
Representative mother particles that can be optimally surface-modified using the apparatus or method of the present invention include various inorganic substances, metals and metal compounds, natural and synthetic organic substances having an average particle diameter of about 0.1 to 100 μm. The average particle size of the child particles used by being dispersed in a liquid such as water is about 0.001 to 10 μm, but a solution in which a solid component solute is dissolved in a liquid or a solid component melt is used. In this case, the particle size of the solid component is not limited. However, without being limited to these materials, various combinations of various materials used in various chemical industries, electricity, magnetic material industries, pharmaceuticals, cosmetics, paints, foods, rubber, plastics, ceramics, etc. Can be applied to the ingredients. However, the apparatus or method of the present invention is particularly suitable for the treatment of pharmaceuticals and toners.
In the treatment method described above, solid particles (base particles) for surface modification are introduced into the impact chamber 8 by opening the on-off valve 17 from the raw material hobber 16 and fine solid particles ( A configuration is adopted in which the dispersion liquid in which the child particles are dispersed is sprayed into the circulation circuit tube 20 through the spray nozzle 22a. However, not only such a treatment method, but also solid particles (mother particles) for surface modification are dispersed in the liquid material referred to in the present invention, such as a dispersion in which the fine solid particles (child particles) are dispersed, and spray nozzles are used. It is good also as a structure supplied in the apparatus via 22a, 22b.

Next, the surface modification treatment of solid particles using the apparatus of the present invention will be specifically described in comparison with a conventional apparatus.
-Examples T-1 to T-3-
[Device used]
The apparatus of the present invention shown in FIGS. 1 to 4 was used. In addition, the dimension of each part was as follows.
・ Turntable diameter: 125mm
-Volume of impact chamber: 0.53 liters-Volume of circulation circuit tube: 1.83 liters-Inner diameter of circulation circuit tube: 22 mm (enlarged part: 33.7 mm)
[Processed powder]
-Mother particles: polystyrene spherical particles (average particle size: 10 μm)
Child particles: titanium dioxide (average particle size: 0.2 μm)
[Processing operations and processing results]
The rotating speed of the turntable 4 was set to 15000 min −1 (98.2 m / sec), and hot air having various temperatures and air volumes shown in Table 1 was supplied into the circulation circuit tube 20 from the supply port 23. Further, an excess amount of circulating gas equivalent to the hot air was discharged from the exhaust port 24 by an ejector pump (not shown).
30 g of the above mother particles were put into the impact chamber 8 from the raw material hover 16. In addition, 3 g of dispersion (10% with respect to the mother particles) in which 15% by weight of the above child particles were dispersed in water was sprayed into the circulation circuit tube 20 from the spray nozzle 22a in 3 minutes. At this time, the flow rate of the compressed air supplied to the spray nozzle 22a was 37 liters / min.
After spraying the dispersion, the operation was continued for another 2 minutes, and the recovered product was observed with a scanning electron microscope. As a result, in any of the examples, it was found that the child particles were particles fixed uniformly on the surface of the mother particles.

-Comparative Example 1-
[Device used]
A hybridization system (NHS-0 type) manufactured by Nara Machinery Co., Ltd. was used. In addition, the dimension of each part was as follows.
・ Turntable diameter: 125 mm
・ Volume of impact chamber: 0.53 liter ・ Volume of circulation circuit tube: 0.13 liter ・ Inner diameter of circulation circuit tube: 22 mm
[Processed powder]
-Mother particles: polystyrene spherical particles (average particle size: 10 μm)
Child particles: titanium dioxide (average particle size: 0.2 μm)
[Processing operations and processing results]
The rotation speed of the turntable was set to 15000 min-1 (98.2 m / sec) as in the above example. In the comparative example, only the shaft seal seal air of 5 liters / min is supplied. Therefore, even if hot air of 40 ° C. is used for this shaft seal, the time required for the calculation is about 7.6. It's time.
In the comparative example, a dispersion containing the same child particles as in the above example was supplied from the opening of the circulation circuit tube using a syringe. That is, 3 g of the dispersion was slowly supplied from the opening of the circulation circuit tube using a syringe over 10 minutes. Thereafter, the operation was continued for another 10 minutes.
After that, the on-off valve for discharging the treated powder was opened, but there was almost no product in the product tank. Therefore, the rotation of the rotating disk was stopped, the front cover was opened, and the circulation circuit tube was also disassembled. As a result, it was found that the mother particles and the child particles adhered to the surface of the rotating disk (impact pin) and the collision ring and the inner surface of the circulation circuit tube.
-Example T-4-
[Device used]
The apparatus of the present invention shown in FIGS. 1 to 4 was used. The dimensions and the like of each part are the same as those in Examples T-1 to T-3.
[Processed powder]
-Core particles: ibuprofen powder (average particle size: 70 μm)
・ Coating material: Phospholipid polymer (dissolved in purified water)
[Processing operations and processing results]
First, 45 g of the ibuprofen powder as the core particle was charged into 255 g of a phospholipid polymer aqueous solution in which 2% by weight of the phospholipid polymer as the coating material was dissolved in purified water, and the liquid (300 g) was supplied to Nara Machinery Co., Ltd. Wet pulverization treatment was performed with Micros (MIC-0 type; “Micros” is a registered trademark), which is a wet pulverizer manufactured by the manufacturer. Thus, ibuprofen was pulverized to about 100 nm and a dispersion liquid uniformly dispersed in the aqueous phospholipid polymer solution was prepared.
Next, the rotational speed of the turntable 4 was set to 16200 min −1 (106 m / sec), and the gas (air) having the temperature and air volume shown in Table 2 was supplied into the circulation circuit tube 20 from the supply port 23. Further, an excessive amount of circulating gas equivalent to this gas was discharged from the exhaust port 24 by an ejector pump (not shown).
Subsequently, the adjusted dispersion was sprayed into the circulation circuit tube 20 from the spray nozzle 22a over 3 hours and 34 minutes. At this time, the flow rate of the compressed air supplied to the spray nozzle 22a was 30 liters / min.
After spraying the dispersion, the operation was continued for another 5 minutes, and the recovered product was observed with a scanning electron microscope. As a result, it was found that if ibuprofen is coated with a phospholipid polymer, it is a granulated composite particle having an average particle diameter of 10 μm or less.

-Comparative Example 2-
Medium fluidized dryer (MSD-100) manufactured by Nara Machinery Co., Ltd., which can continuously dry the slurry of the same dispersion as above and take out the solid content dispersed in the slurry in the size of primary particles. To be processed.
In this case, since the polymer was contained in the dispersion, the medium particles were completely coated with the dispersion, and the product (ibuprofen coated with the phospholipid polymer) could not be recovered.
Moreover, the same dispersion liquid as the above was subjected to a drying treatment using a spray dryer (L-8i) manufactured by Okawara Chemical Co., Ltd. and a freeze-drying apparatus (FDU-2100) manufactured by Tokyo Rika Kikai Co., Ltd.
In this case, the particle size of the obtained product was large (30 μm or more even by the spray drying method), and fine composite particles equivalent to Example T-4 could not be obtained.

According to the solid particle surface modifying apparatus or surface modifying method according to the present invention described above, the solid particles can be efficiently dried or cooled according to the type of the liquid, and the solid particles are excellent in productivity and good. Surface modification treatment of various solid particles used in various chemical industries, electricity, magnetic materials industry, pharmaceuticals, cosmetics, paints, foods, rubber, plastics, ceramics, etc. Can be widely used for quality.

Claims

In the impact chamber, a rotating disk with impact pins is arranged, and a collision ring is arranged along the outermost raceway surface of the impact pins with a certain space therebetween, and the impact pins rotate. A circulating circuit tube for guiding and circulating the treated powder together with the air flow generated by the above-mentioned circuit. One opening of the circulating circuit tube is opened in a part of the collision ring, and the other opening is located near the center of the rotating disk. A spray nozzle is provided to be opened in the front cover, supplying a liquid material to any one of the front cover, the collision ring, or the circulation circuit tube, and a heating medium, a cooling medium, or a drying medium is supplied to an appropriate position of the circulation circuit tube. A solid particle surface reforming apparatus comprising a supply port for exhausting and an exhaust port for discharging excess circulating gas.
2. The solid particle according to claim 1, wherein the supply port is provided in the circulation circuit tube, and the exhaust port is provided in the circulation circuit tube located on the downstream side of the supply port. Surface modification equipment.
The surface modification apparatus for solid particles according to claim 1 or 2, wherein a part of the circulation circuit tube is enlarged to form an enlarged portion.
4. The solid particle surface reforming apparatus according to claim 3, wherein the enlarged portion of the circulation circuit tube is formed between the downstream side of the supply port and the upstream side of the exhaust port.
5. The surface modification device for solid particles according to claim 1, wherein a powder recovery device is connected to the exhaust port.
The spray nozzle for supplying the liquid material is provided at the upstream end of the circulation circuit tube, the supply port is provided at a portion of the circulation circuit tube located immediately downstream of the spray nozzle, and the downstream side of the supply port. The surface modification of the solid particles according to any one of claims 1 to 5, wherein the exhaust port is provided in a portion of the circulation circuit tube at a position relatively close to the upstream end side. Quality equipment.
6. The surface modification apparatus for solid particles according to claim 1, wherein a spray nozzle for supplying a liquid material is provided at a downstream end of the circulation circuit tube.
Using the solid particle surface modifying apparatus according to any one of claims 1 to 7, the solid particles to be subjected to surface modification are put into the apparatus separately from the liquid material, and the surface modification of the solid particles is performed. A method for modifying the surface of solid particles, characterized by comprising:
Using the solid particle surface modification device according to any one of claims 1 to 7, the solid particles to be surface-modified are dispersed in the liquid and charged into the device through the spray nozzle. A method for modifying the surface of a solid particle, comprising performing surface modification of the solid particle.