JPS6152736B2 - - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for manufacturing ultrafine capsules filled with a high melting point substance and an apparatus for manufacturing the same.

The present applicant disclosed in Japanese Patent Application No. 122,695/1982 a method and apparatus for manufacturing capsules that can continuously mass-produce ultra-fine capsules. In this method, ultrafine capsules are manufactured by extruding the capsule filling material and the coating material from the tip of a double nozzle into a capsule coagulating liquid whose flow rate is increased by pressure. The coagulating liquid is introduced into the closed channel, and its flow rate can be freely controlled by the discharge capacity of the pump.

However, with this conventional method and apparatus, there was a problem in that it was extremely difficult to reduce the particle size of capsules filled with a high melting point substance to 2 mmφ or less. This is because when the jet stream pushed out from the nozzle into the coagulating liquid cools rapidly, it becomes difficult to cut, making it difficult to obtain uniform capsules, and the nozzle is more likely to become clogged. It was hot.

In view of the above circumstances, the inventors of the present application focused on the problem of the cooling temperature and cooling time of the jet flow, and believed that if these could be freely adjusted, ultrafine encapsulation of high melting point substances would be possible. As a result of our studies, we have completed the present invention.

SUMMARY OF THE INVENTION An object of the present invention is to provide a method for obtaining capsules filled with a high melting point substance and an apparatus for producing the same, which solves the above-mentioned problems by preventing rapid cooling of the jet flow and thereby improving the cutting of the jet flow.

Hereinafter, the method and apparatus according to the present invention will be explained based on the accompanying drawings.

The components up to the stage of forming the jet flow into a spherical shape include a capsule filling material separation introduction chamber 1;
Capsule film substance introduction chamber 2 and encapsulation adjustment liquid introduction chamber 3 whose temperature can be set artificially
, a capsule coagulating liquid introducing chamber 4, and a hopper section 5, a pipe 9 connected to a capsule filling material tank 8 is opened in the capsule filling material introducing chamber 1, and There are six capsule filling material nozzles 11 in one row, that is, 36 capsule filling material nozzles 11, and the capsule coating material chamber 2 includes:
A pipe 13 connected to the capsule coating substance storage tank 12 is opened, and the chamber bar 2 further has a pipe 13 concentrically surrounding the outer circumference of each capsule filling nozzle 11 extending downward through the partition wall. However, the capsule film material nozzle 15 is arranged in series.
Next, a pipe 17 connected to the capsule coagulation liquid tank 16 is provided to the encapsulation adjustment liquid introduction chamber 3 whose temperature can be set artificially.
The end of the pipe 20 is opened via an encapsulated adjustment liquid tank 21 which is installed in the middle of the pipe 20 where the temperature is set artificially, and the chamber bar 3 is provided with a tank 21 that penetrates the partition wall. For each extending coating substance nozzle 15, there is further provided a nozzle 22 for the encapsulation conditioning liquid having an artificially set temperature, which surrounds it in concentric circles on the outside of its periphery. A triple nozzle having such a configuration is arranged, and the lower end of this triple nozzle is connected to the upper end opening 2 of each of the same number of capsule forming tubes 23 as the triple nozzle.
3a, and next, in this coagulation liquid introduction chamber 4, the end of the capsule coagulation liquid return pipe 17, which forms a closed circuit from the capsule coagulation liquid storage tank 16 through the heat exchanger 24, is open. has been done. Further, this capsule coagulating liquid chamber 4 is provided with a hopper 5 that can be detachably attached, and this hopper 5 has the following features:
The lower end 23b of each of the capsule forming tubes 23 is open, and the lower end 5 of the hopper 5 is opened.
a opens onto the capsule coagulation liquid storage tank 16. This tank 16 has such a structure in which a conveyor 25 for separating capsules and a capsule storage box 26 are provided.

Next, an embodiment of a method for continuously mass-producing target ultra-fine microcapsules of a high melting point substance using the capsule manufacturing apparatus according to the present invention will be described in detail below.

In this example, palm wax (mp86°) is used as the capsule filling material, and gelatin 20 is used as the capsule coating material.
%, purified water 80%, and liquid paraffin was used for both the encapsulation adjustment liquid and capsule coagulation liquid whose temperature was artificially adjusted.

First, as a preliminary preparation, the capsule filling material separation chamber 1, the capsule coating material separation chamber 2, the encapsulation adjustment liquid introduction chamber 3 whose temperature can be set artificially, and the capsule coagulation liquid chamber 4 are separated, and then the coagulation liquid is separated. The discharge rate of the pump is adjusted to such an extent that the circulating flow rate of the capsule membrane material does not overflow from the upper flange of the chamber bar.
Next, liquid paraffin, which is a coagulating liquid, is set in a heat exchanger 24 to a predetermined temperature. Next, palm wax (mp86°) is placed in the capsule filling material tank 8, and a mixed solution of 20% gelatin and 80% purified water is placed in the capsule coating material tank 12. In this case, palm wax, which is the capsule filling material, is pumped into the metering pump 10, which is preset to a predetermined discharge rate.
The capsule filling material is fed into the pipe 9 and introduced into the separating chamber 1. Next, a mixed solution of 20% gelatin and 80% purified water, which is a coating material, is also introduced into the coating material chamber 2 by the metering pump 14, which is set in advance at a predetermined discharge rate. Next, liquid paraffin, which has been artificially set at a higher temperature than the liquid paraffin of the coagulation liquid to be refluxed, is introduced into the encapsulation adjustment liquid introducing chamber 3 from the reflux adjustment liquid tank 21 through the pipe 20. When each chamber bar is filled with liquid and the liquid starts to be discharged from the triple nozzle, they are attached to the capsule coagulation liquid introduction chamber 4. In this device, the discharge amount of the pump 18 is adjusted so that the flow rate of the coagulating liquid flowing down the capsule forming tube 23 becomes a predetermined value.Since the coagulating liquid introducing chamber 4 is a closed circuit, the flow rate of the liquid paraffin is adjusted to a predetermined value. is pump 1
By changing the discharge amount of 8, the flow velocity can be freely changed. In the case of this example, palm wax, which is the capsule filling material, flows down at a constant speed through 36 capsule filling material nozzles 11, and a mixture of 20% gelatin and 80% purified water, which is introduced into the capsule membrane material introduction chamber 2, flows down at a constant speed through 36 capsule filling material nozzles 11. The solution also includes 36 capsule filling material nozzles 11 and film material filling nozzles 1
The encapsulation adjustment liquid flowing down at a constant speed between the encapsulation adjustment liquid chamber 3 and the encapsulation adjustment liquid chamber 3 whose temperature can be set artificially is also integrated at the lower end of the triple nozzle. The core cylindrical composite jet is discharged into the downward flow of liquid paraffin in the capsule-forming tube 23. As the composite jet flow discharged here descends, it gradually becomes constricted due to the interfacial tension that acts between the liquids that make up the composite jet flow, forming approximately spherical droplet-shaped capsules. go. The capsules thus formed are cooled as they descend through the liquid paraffin, yielding the desired perfectly spherical, seamless microcapsules. The seamless microcapsules formed through such a process flow down into the hopper 5 together with the liquid paraffin, are collected, and fall onto a net-like separation conveyor 25 below the outlet of the hopper 5. The mesh of the net used in this net-shaped conveyor 25 is smaller than the diameter of the capsules, so the microcapsules 27 obtained here are conveyed on the net without passing through the mesh, and are removed by a scraper. The capsule is scraped off and stored in the capsule storage container 26. Liquid paraffin, which is a coagulating liquid, falls through the mesh into the coagulating liquid storage tank 16 and is circulated again for use.

As described above, according to the present invention, the cooling time of the nuclear material is extended and the jet flow is better cut, so that ultrafine capsules of high melting point material with uniform particle sizes of 10 mm to 50 μφ can be obtained. Excellent effects are produced, such as the phenomenon that the nozzle is cooled too much and the core material clogs the tip of the nozzle.

[Brief explanation of the drawing]

FIG. 1 is a simplified explanatory diagram showing the internal structure of the capsule manufacturing apparatus according to the present invention, and FIG. 2 is a jet flow of each liquid from three consecutive nozzles into the capsule forming tube through the lower end of the core. An enlarged view showing the state in which a person is injected as
FIG. 3 is a plan view showing the installed state of the nozzle. 1...Capsule filling material chamber bar, 2...Capsule coating material chamber bar, 3...Encapsulation adjustment liquid introduction chamber bar for artificially setting temperature, 4...
... Capsule coagulation liquid introduction chamber, 5 ... Hopper, 8 ... Capsule filling material tank, 9, 13,
17, 20...pipe, 10, 14, 18, 19
... pump, 11 ... nozzle for capsule filling material, 12 ... capsule coating material storage tank, 15
... Nozzle for capsule coating material, 16 ... Capsule coagulation liquid tank, 21 ... Encapsulation adjustment liquid tank, 22 ... Encapsulation adjustment liquid nozzle, 23 ...
Capsule forming tube, 24...heat exchanger, 25...conveyor, 26...capsule storage box.

Claims (1)

[Scope of Claims] 1. A composite in which a capsule coating material is in contact with the periphery of a capsule filling material, and further, another capsule coagulating liquid whose temperature is set higher than that of the capsule coagulating liquid is in contact with the periphery of the capsule coating material to form an integral body. 1. A method for producing microcapsules filled with a high melting point substance, which comprises a step of extruding a jet flow into a falling capsule coagulating liquid, and a step of increasing the speed of the falling capsule coagulating liquid by forced means. 2. Claim 1, wherein the forcing means is based on pressure controlled by the discharge amount of the pump.
A method for producing microcapsules filled with a high melting point substance as described in . 3 capsule fill material chamber 1 to which capsule fill material tank 8 is connected via pump 10;
and the capsule film material storage tank 12 is connected to the pump 1.
The capsule membrane material chamber 2 and the capsule coagulation liquid tank 16 connected via the pump 18
and a capsule coagulating liquid introducing chamber 4 which is connected via a heat exchanger 24 to form a sealed path, and a hopper 5, and the capsule filling material chamber 1 includes a plurality of capsule filling material nozzles 11, Further, the capsule coating material chamber bar 2 has a number of capsule coating material nozzles 15 corresponding to the nozzles 11 for the capsule filling material, and the coagulating liquid introduction chamber bar 4 has capsule coating material nozzles 15 in a number corresponding to the capsule coating material nozzles 15. Forming tube 23
Each of the capsule filling material nozzle 11, capsule coating material nozzle 15, and capsule forming tube 23 is provided in each chamber bar, and a nozzle and a forming tube extending through the bottom of the chamber bar are respectively provided. They are connected so that the centers of their diameters are on the same line, and the lower end of the capsule forming tube 23 in the coagulation liquid introduction chamber 4 is opened into the hopper 5, and the lower end of the hopper 5 is inserted into the capsule coagulation liquid tank 16. Specifically, in a capsule manufacturing apparatus in which the tank 16 is provided with a device for separating capsules and coagulation liquid, a reflux pipe 17 for capsule coagulation liquid is used.
A pump 19 is installed in the middle of the pipe 20 that is branched out.
An encapsulation adjustment tank 21 for storing the encapsulation adjustment liquid is provided, and an encapsulation adjustment liquid introduction chamber 3 to which a pipe 20 extending from the tank 21 is connected and whose temperature can be set artificially is provided, and the encapsulation adjustment liquid is introduced. The apparatus for manufacturing microcapsules filled with a high melting point substance is characterized in that the nozzle 22 provided on the chamber bar 3 is configured to further surround the outside of the nozzle 11 and the nozzle 15.