JPS621288B2 - - Google Patents

Description

[Detailed description of the invention]

The present invention relates to a method and apparatus for manufacturing ultrafine capsules by extruding a capsule filling material and a coating material into a coagulating liquid whose flow is sped up by pressure. In conventional capsule manufacturing equipment, for example,
-As stated in Publication No. 8875, the entire circulation circuit of the coagulating liquid in the capsule is open, and therefore there is a limit to the adjustment of the flow rate of the coagulating liquid, so the diameter of what is called an ultra-fine capsule is about 1 mm to 50 μm. It was impossible to mass produce these things continuously. The inventors of the present application have conducted various studies on conventional capsule manufacturing equipment, and have now developed a method and equipment that can easily and continuously manufacture large quantities of ultrafine capsules at an excellent speed. The capsule manufacturing apparatus according to the present invention has a feature that the flow rate of the coagulation liquid can be determined by the discharge capacity of the coagulation liquid supply pump, since the inside of the chamber bar in which the capsule forming tube etc. are installed is sealed. ing. That is, it is possible to increase the flow rate of the coagulating liquid by changing the discharge amount of the pump, and it is possible to increase the flow rate to a speed that could not be achieved with conventional devices. This affects the particle size of the capsules formed,
As a result, it became possible to obtain extremely small capsules. Another feature is that in addition to speeding up the flow of the coagulation liquid, by using multiple nozzles and capsule forming tubes, it is possible to manufacture extremely large amounts of ultra-fine capsules at once. be. The present invention aims to provide a method and apparatus for obtaining such microcapsules. To achieve the above object, the present invention provides a method for mass-producing capsules by extruding a capsule filling material and a coating material from the tips of a plurality of double nozzles into a refluxing coagulating liquid. Capsules are manufactured by forcibly increasing the flow rate and converting the jet flow of the capsule filling material and coating material into minute droplets, which are extruded from the tips of a plurality of double nozzles into the coagulation liquid. The apparatus for carrying out the above method also includes a capsule filling material chamber to which the capsule filling material storage tank is connected via a pump, and a capsule coating material chamber to which the capsule coating material storage tank is connected via a pump. It is composed of a liquid chamber, a capsule coagulation liquid separation chamber to which a capsule coagulation liquid storage tank is connected via a pump and a heat exchanger, and a hopper section connected to the capsule coagulation liquid separation chamber, and a hopper part connected to the capsule coagulation liquid separation chamber; There are multiple capsule filling nozzles in the separation chamber, capsule coating material nozzles corresponding to the number of capsule filling nozzles in the capsule coating material separation chamber, and capsule coating material nozzles corresponding to the capsule coating material nozzles in the coagulation liquid separation chamber. a number of capsule-forming tubes are provided, and the capsule-coating material nozzle surrounds the outside of the capsule-filling material nozzle in the capsule-coagulating material separation chamber, and the lower end of the nozzle is connected to the capsule-forming tube in the capsule-coagulating liquid separating chamber. The lower end of the capsule forming tube is opened into the hopper, and the lower end of the hopper is opened into a coagulation liquid storage tank, and the tank is equipped with a device for separating the capsules and the coagulation liquid. It is something that has been established. Hereinafter, the configuration of the apparatus according to the present invention will be explained with reference to the accompanying drawings. As shown in FIG. 1, this device is equipped with a lid 4a and an inlet 4b on the top surface where a capsule filling material storage tank 1 is connected by a pipe 3 via a metering pump 2 with a variable speed gear. A capsule filling material chamber 4, a capsule coating material separation chamber 8 with an inlet 8a to which a capsule coating material storage tank 5 is connected by a pipe 7 via a variable speed gear metering pump 6, and a coagulation liquid storage. a closed-circuit coagulation liquid separation chamber 13 equipped with an inlet 13a connected to the tank 9 by a pipe 12 via a metering pump 10 with a variable speed gear and a heat exchanger 11 for controlling the temperature of the coagulation liquid; It consists of a hopper section 14, which can be separated from each other. The capsule filling material separating chamber 4 has six rows of capsule filling material nozzles 15 extending through the bottom to the capsule coating material separating chamber 8, and each row has six capsule filling material nozzles 15, that is, a total of 36 capsule filling material nozzles 15. Similarly to the capsule filling material nozzles 15, capsule coating material nozzles 16 in the same row are arranged in the capsule coating material separation chamber 8 located below the capsule coating material nozzles 15 so as to cover the lower portions of the capsule filling materials 15, respectively. The lower end of each of the capsule coating substance nozzles 16 is provided so as to penetrate through the bottom and further into the closed circuit capsule coagulation liquid separation chamber 13 located below. In this closed-circuit coagulation liquid separation chamber 13, capsule forming tubes 17 in the same number and row as the capsule coating substance nozzles 16 are disposed, and the top openings of each of the capsule forming tubes 17 have the above-mentioned openings. The lower end portions of the capsule coating material nozzles 16 are provided so as to be located respectively. Continuously like this,
The 36 capsule filling material nozzles 15, capsule coating material nozzles 16, and capsule forming tubes 17 are arranged so that the centers of their respective diameters are on the same line. Furthermore, the lower end of each of the capsule forming tubes 17 passes through the bottom and opens into the hopper 14.
The lower end opening 14a of 4 faces the capsule coagulation liquid storage tank 9. Next, a net-shaped separating conveyor 19 is attached to this capsule coagulating liquid storage tank 9 to separate the capsules and the coagulating liquid. 18 is a scraper. Then, the storage container 20 of the capsules 21 separated from the coagulated liquid during conveyance by the net-like separation conveyor 19 is moved to the scraper 1.
It is located under 8. In this case, the mesh of the net-shaped separating conveyor 19 can be easily replaced depending on the size of the capsules 21 to be manufactured, and by changing the speed of the conveyor 19, it is possible to respond to fluctuations in the amount of containers produced. It's like this. The configuration of the capsule manufacturing apparatus according to the present invention has been described above, and the vibration device attached to a part of this apparatus in an attachment type will be explained below. This device is used only when creating capsules by applying vertical vibration to the capsule filling material.
To explain this with reference to FIG. 4, in this case, instead of the lid 4a of the capsule filling material separation chamber 4, the same arrangement as the nozzle 15 of the capsule filling material,
A lid 30 provided with several holes is used. A vibrating rod 32 for vibrating the capsule filling material is passed through a hole 31 provided in the lid 30, and the top part is attached to a diaphragm 33 and the bottom part is inserted into the capsule filling material nozzle 15, respectively. A vibrator 34 is attached to this diaphragm 33, and a vibrating rod 32
The amplitude and frequency of the vibrations can be adjusted depending on the size of the capsule and the required number of vibrations per second. 4b is an inlet for capsule filling material. FIG. 5 shows a partially enlarged view of the vibrating rod, the vibrating rod 3 whose lower end is inserted into the capsule filling material nozzle 15.
2 shows a structure for preventing leakage of the filling material from inside the filling material nozzle 15 due to vertical movement of the capsule filling material nozzle 15 and a positional relationship between the vibrating rod 32 and the capsule filling material nozzle 15. 35 in the figure is a sealing material 36
This is a cover to prevent movement of the As mentioned above, this vibration device is used only when creating capsules by applying vibration to the capsule filling material in this device. Next, a method for continuously mass-producing the desired ultrafine capsules using the capsule manufacturing apparatus according to the present invention will be described in detail by way of an example. In this example, purified vegetable oil was used as the capsule filling material, a mixed solution of 20% gelatin, 2.2% sorbitol, and 77.8% purified water was used as the capsule coating material, and liquid paraffin was used as the coagulation liquid. First, as a preliminary preparation, the capsule filling material separation chamber 4 and the capsule coating material separation chamber 8 are separated from the capsule coagulation liquid separation chamber 13, and then the circulating flow rate of the coagulation liquid is adjusted to the capsule coating material chamber 8.
The discharge amount of the pump 10 is adjusted to such an extent that it does not overflow from the upper flange of the pump 10. Next, liquid paraffin, which is a coagulating liquid, is set in a heat exchanger 11 to a predetermined temperature. After completing the above pre-operation, the capsule filling material tank 1 is filled with purified vegetable oil, and the capsule coating material tank 5 is filled with a mixed solution of 20% gelatin, 2.2% sorbitol, and 77.8% purified water. In this case, the refined vegetable oil serving as the capsule filling material is fed through the pipe 3 by the metering pump 2, which is set in advance at a predetermined discharge rate, and is introduced into the capsule filling material separating chamber 4 through the inlet 4b. Next is 20% gelatin, which is the coating material, 2.2% sorbitol, and refined oil.
A 77.8% mixed solution is also fed into the pipe 7 by a metering pump whose discharge rate has been set in advance, and introduced into the capsule membrane material separating chamber 8 through the inlet 8a. Here, the capsule filling material separation chamber 4 and the capsule coating material separation chamber 8 are filled with their respective liquids, and the capsule coating material nozzle 16 is filled with the respective liquids.
When more liquid begins to be discharged, at this point the capsule is attached to the closed-circuit coagulation liquid separating chamber 13.
In this case, the capsule filling material nozzle 15, capsule coating material nozzle 16, and capsule forming tube 17 are arranged as shown in FIG. Next, a pump 10 is used to adjust the flow rate of the liquid paraffin, which is a coagulating liquid, flowing down the capsule forming pipe 17 to a predetermined speed.
Adjust the discharge amount. That is, since the coagulation liquid separation chamber 13 is a closed circuit, the flow rate of the liquid paraffin can be freely changed by changing the discharge amount of the pump 10.
Refined vegetable oil, which is a filling material introduced into the capsule filling material chamber 4, flows down through 36 capsule filling material nozzles 15 at a speed of about 10 m/sec, and is also introduced into the capsule filling material separation chamber 8, which is a membrane film. A mixture of 20% gelatin, 2.2% sorbitol, and 77.8% purified water also flows down at a speed of about 10 m/sec between the 36 filler material nozzles 16, and both liquids flow at the lower end of the capsule membrane material nozzles 16. and is discharged as a concentric cylindrical composite jet into the downward flow of liquid paraffin in the capsule-forming tube 17. The composite jet stream discharged here, as it descends, contains liquid paraffin as a coagulating liquid, 20% gelatin as a film material, 2.2% sorbitol,
The interfacial tension acting between the mixed liquid of 77.8% purified water and the purified vegetable oil serving as the capsule filling material gradually creates a constriction, resulting in capsules 21 in the shape of approximately spherical drops.
is formed. This capsule 21 is then cooled while descending in liquid paraffin, thereby obtaining the desired perfectly spherical, seamless, ultra-fine filled capsule. This device can do this all at once with 36 filling and coating nozzles and 36 forming tubes. The seamless ultrafine capsule formed as described above is
It flows down into the hopper 14 together with liquid paraffin,
They are collected and fall onto a net-shaped separation conveyor 19 below the discharge port 14a of the hopper 14. The mesh of the net used in this net-like conveyor 19 is smaller than the diameter of the capsule 21.
Therefore, the capsules 21 are conveyed along the net without passing through the mesh, are scraped off from the net by the scraper 18, and are stored in the capsule storage container 20. Liquid paraffin, which is a coagulating liquid, falls into a coagulating liquid storage tank 9 below the mesh and is circulated again for use. The method described above is a method for obtaining the desired capsule using this device, and is a method that is performed without applying vibration to the filling material. Next, a method of manufacturing a filling material by applying vibration to it using this apparatus will be described below. When this method is used, an attachment-type vibrating device, that is, a vibrating machine, a vibrating plate, a vibrating rod, and a lid 4 of a capsule filling material separating chamber, as explained in the section of the configuration of the present device, are used.
Instead, a lid 30 as shown in FIGS. 4 and 5, which has holes equal to the number of nozzles of the filling material, and a sealing material 36 for fixing the lid are set. Next, in the same manner as in the above method without vibration of the capsule filling material, purified vegetable oil as the filling material was added to the capsule filling material separation chamber 4, and 20% gelatin, 2.2% sorbitol, and purified water as the capsule coating material.
The 77.8% mixed solution is introduced into the capsule membrane filling material separation chamber 8, respectively, and after each chamber is filled with liquid, these are attached to the capsule coagulation liquid separation chamber 13. After that, the flow rate of the coagulating liquid flowing down the capsule forming tube 17 is adjusted to a predetermined value by the pump 10. Next, in order to make the capsules into a predetermined uniform size, the purified vegetable oil serving as the filling material is vibrated by a vibrating rod 32 inserted into the capsule filling nozzle 15. Vibration rod 3
2 is partially inserted into the filling material nozzle 15, so that the flow of refined vegetable oil, which is the filling material, inside the filling material nozzle 15 is completely caused by the vibration of the vibration rod 32 due to the vertical vibration of the vibration rod 32. It begins to vibrate in accordance with the number. That is, filling substance nozzle 1
Refined vegetable oil, which is the filling material discharged from 5, becomes faster or slower. The effect of this speed variation directly affects the coating material, which is a mixture of 20% gelatin, 2.2% sorbitol, and 77.8% purified water, creating a constriction in the jet that matches the vibration frequency of the vibrating rod 32, making it extremely uniform. A seamlessly filled capsule 21 can be obtained. Thereafter, the procedure is exactly the same as in the method for obtaining capsules without vibration described above. When the capsule particle size is relatively large, 1 mm or more, extremely uniform, seamlessly filled capsules can be obtained by applying vibration. Next, the experimental results using this device are shown in the table.

[Table] Next, the effects of this device are listed below. (1) The flow rate of the coagulating liquid can be adjusted simply by changing the gear of the metering pump, making it extremely easy to operate.Furthermore, with conventional methods using a head, the flow rate is inevitably limited by the head of the device, but with this device, This does not happen, and the flow rate of the capsule coagulating liquid is determined by the pump's discharge capacity, so the device is compact. (2) Capsules with a diameter of 10mm to 50μ can be produced. (3) It is possible to manufacture ultrafine capsules with a high degree of freedom in coating rate and coating formulation. (4) Since it is not a batch type, production efficiency is extremely high. (5) Since it has a large number of nozzles and formation tubes, when using the 36 nozzles shown in this example, it is possible to obtain a maximum of 1.73 million capsules per second. Capsules can be mass-produced continuously.

[Brief explanation of the drawing]

FIG. 1 is a diagram showing the manufacturing principle of the ultrafine capsule manufacturing apparatus according to the present invention. FIG. 2 is a partially enlarged view showing the state in which the filler material and the coating material are formed into spherical droplets in the downward flow of the capsule forming tube. FIG. 3 shows one embodiment, and is a plan view showing a state in which 36 nozzles are arranged in a filling material separating chamber bar with the lid removed. Figures 4 and 5 show a vibration device that is attached to a part of this equipment in an attachment type when manufacturing capsules by applying vibration to the filling material. FIG. 5 is a partial cross-sectional view showing a state in which a vibrating rod connected to a vibrating plate equipped with a vibrator is inserted into each of the filling material nozzles provided in the separation chamber bar, and FIG. FIG. 3 is an explanatory diagram showing an enlarged structure of the attachment part. In Figures 1, 2, and 3, 1... Capsule filling material storage tank, 2... Metering pump with variable speed gear, 3... Pipe, 4... Capsule filling material chamber bar, 5... Capsule film material storage. Tank, 6... Variable speed gear metering pump, 7... Pipe, 8... Capsule coating material separation chamber, 9
... Coagulation liquid storage tank, 10 ... Metering pump with variable speed gear, 11 ... Heat exchanger, 12 ... Pipe, 13 ... Coagulation liquid separation chamber, 14 ... Hopper section, 15 ... Capsule filling material Nozzle, 1
6... Capsule film material nozzle, 17... Capsule forming tube, 18... Scraper, 19... Net-like separation conveyor, 20... Capsule storage container, in FIGS. 4 and 5, 30... hole Lid provided, 31... Hole provided in the lid, 32... Vibration rod, 33... Vibration plate, 34... Vibrator, 35...
Cover, 36...Sealing material.

Claims (1)

[Claims] 1. A method for mass-producing capsules by extruding a capsule filling material and a coating material from the tips of a plurality of double nozzles into a refluxing coagulating liquid, in which the flow rate of the coagulating liquid is forced by pressure. The ultra-fine capsule is characterized in that the jet flow of the capsule filling material 38 and the coating material 39 extruded from the tips of a plurality of double nozzles into the coagulating liquid is made into minute droplets. A capsule manufacturing method that allows continuous mass production. 2. A capsule filling material chamber 4 to which the capsule filling material storage tank 1 is connected via a pump 2; a capsule coating material separation chamber 8 to which the capsule coating material storage tank 5 is connected via a pump 6; The coagulation liquid storage tank 9 is composed of a capsule coagulation liquid separation chamber 13 connected to the capsule coagulation liquid separation chamber 13 via a pump 10 and a heat exchanger 11, and a hopper section 14 connected to the capsule coagulation liquid separation chamber 13. A plurality of capsule filling nozzles 15 are provided in the substance separation chamber 4, and a capsule coating material separation chamber 8 is provided.
A number of capsule coating material nozzles 16 corresponding to the number of capsule filling nozzles 15 are provided in the chamber, and a number of capsule forming tubes 17 corresponding to the number of capsule coating material nozzles 16 are provided in the coagulation liquid separating chamber 13. In the liquid chamber bar 8 the capsule coating material nozzle 16 is connected to the capsule filling material nozzle 1.
The lower end of the nozzle 16 faces the upper end of the capsule forming tube 17 within the capsule coagulating liquid separation chamber 13, and the lower end of the capsule forming tube 17 is opened into the hopper 14. At the same time, the lower end of the hopper 14 is exposed into the coagulation liquid storage tank 9, and the tank 9 is equipped with a device for separating the capsules and the coagulation liquid, thereby making it possible to continuously mass-produce ultra-fine capsules. Capsule manufacturing equipment. 3 a capsule filling material chamber 4 to which the capsule filling material storage tank 1 is connected via a pump 2; a capsule coating material separation chamber 8 to which the capsule coating material storage tank 5 is connected via a pump 6; The coagulation liquid storage tank 9 is composed of a capsule coagulation liquid separation chamber 13 connected to the capsule coagulation liquid separation chamber 13 via a pump 10 and a heat exchanger 11, and a hopper section 14 connected to the capsule coagulation liquid separation chamber 13. A plurality of capsule filling nozzles 15 are provided in the substance separation chamber 4, and a capsule coating material separation chamber 8 is provided.
A number of capsule coating material nozzles 16 corresponding to the number of capsule filling nozzles 15 are provided in the chamber, and a number of capsule forming tubes 17 corresponding to the number of capsule coating material nozzles 16 are provided in the coagulation liquid separating chamber 13. In the liquid chamber bar 8 the capsule coating material nozzle 16 is connected to the capsule filling material nozzle 1.
5, the lower end of the nozzle 16 faces the upper end of the capsule forming tube 17 within the capsule coagulating liquid separating chamber 13, and the top of the nozzle 16 is connected to a diaphragm 33 installed outside the chamber bar. inserting the rod 32 into the capsule fill material nozzle 15;
Furthermore, the lower end of the capsule forming tube 17 is connected to the hopper 1.
4 and the lower end of the hopper 14 faces into the coagulation liquid storage tank 9.
A capsule manufacturing device capable of continuously mass-producing ultra-fine capsules, characterized in that it is equipped with a device for separating capsules and coagulation liquid.