JP2018051421A - Microcapsule manufacturing equipment - Google Patents

Abstract

A microcapsule manufacturing apparatus capable of maintaining a small particle size without bonding microcapsules discharged into a continuous phase to each other. A shaft 2 that rotates by a motor 3 is supported through the center of a base 1, and a turntable 4 is fixed to an upper end of the shaft 2, and a fixing tool 5 is provided on the turntable 4, and this fixing is performed. The storage tank 6 that stores the continuous phase m1 in the tool 5 is fixed so as not to move. In a fixed state, the position of the fixture 5 is determined such that the center O1 of the turntable 4 and the center O2 of the storage tank 6 are eccentric. [Selection] Figure 1

Description

  The present invention relates to a method for producing microcapsules used as food, pharmaceuticals, cosmetics, feed for aquaculture fry, and the like.

  Microcapsules of water-soluble polymers such as gelatin, agar, carrageenan, pectin, and alginic acid containing them to prevent or prevent oxidation and deterioration of flavors, sweeteners, vitamins, drugs, foods, etc. To be done.

  For microencapsulation, a solution (dispersed phase) of a water-soluble polymer is dispersed in a spherical shape in a liquid (continuous phase) that does not mix with the solution. This method is roughly divided into a liquid dispersion method and a liquid dropping method.

  In Patent Document 1, as a dispersion method in liquid, when producing microcapsules of food such as royal jelly or propolis extract, gelatin and maltose are mixed in the presence of water, and the food is added to this mixture. Addition and granulation in oil are disclosed.

  In Patent Document 2, as a dropping method in liquid, a nozzle is immersed in a hydrophobic solvent maintained at a temperature equal to or higher than the gelling temperature of gelatin, and an aqueous gelatin solution in which a chemical is dispersed or dissolved in the hydrophobic solvent is discharged from this nozzle. A method is disclosed. This Patent Document 2 also describes that the aqueous gelatin solution discharged by moving the nozzle in the horizontal direction and the vertical direction is sheared into droplets.

  In Patent Document 3, the lower end of the nozzle is immersed in a dropping tank equipped with a stirrer, and in this state, the gelatin aqueous solution is discharged from the lower end of the nozzle into the hydrophobic solvent in the dropping tank, and then the nozzle is moved to the hydrophobic solvent. It is disclosed to raise from In Patent Document 3, droplets are formed in the same manner as Patent Document 2 by moving the nozzle up and down.

  In Patent Document 4, it is difficult to mix seamless capsule film liquid from the outermost nozzle of a triple nozzle with a triple structure arranged concentrically, and hydrophilic substance liquid from the innermost nozzle and water from an intermediate nozzle. A method for producing a seamless capsule in which a viscous liquid is simultaneously extruded into a cooling liquid is disclosed. Patent Document 4 also discloses that a continuous phase around a nozzle is caused to flow by a pump or the like.

  Patent Document 5 discloses a method of manufacturing a seamless capsule by dropping a multi-layer droplet into a curable liquid using a vibrating concentric multiple nozzle.

  Patent Document 6 discloses a method of encapsulating a continuous phase by using a cooled gas, not a liquid, and spraying an aqueous gelatin solution into the gas.

  Patent Document 7 discloses the contents of dropping the produced microcapsule onto a rotating disk in order to prevent the cured microcapsule from being fused and deformed.

JP-A-10-136912 JP 60-215365 A JP 2010-77062 A JP-A-5-31352 JP-A-9-155183 JP-A-5-71215 Japanese Patent Laid-Open No. 3-127819

  When the gelatin aqueous solution is discharged from the nozzle, the discharged gelatin solution is not gelled, and in this state, the gelatin particles come into contact with each other and coalesce (bond), or the shearing force acting on the discharged droplets On the contrary, there is a problem that the particle size becomes small and the particle size distribution becomes large.

  For this reason, in the prior art described above, measures are taken such as giving vibration to the nozzle, reciprocating the nozzle up and down or horizontally, and making the continuous phase a cooled gas. No results have been obtained.

  In addition, in the method of forming droplets by stirring without using a nozzle or the method of spraying in the air as in Patent Document 6, the particle size distribution of the formed microcapsules spreads to several μm to several thousand μm, It is impossible to efficiently produce a macrocapsule having a target particle size.

  In order to solve the above problems, the present invention provides a microcapsule manufacturing apparatus in which a nozzle that discharges a dispersed phase solution into a liquid that becomes a continuous phase in a storage tank, and the storage tank rotates on a turntable. It is set as the structure mounted in the state where the rotation center of the stand and the center of the storage tank are eccentric.

  Moreover, as a microcapsule manufacturing apparatus according to the present invention, a separation tank is disposed adjacent to the storage tank, and a continuous phase liquid containing the microcapsules in the storage tank is taken into the separation tank. It is also conceivable to return the continuous phase liquid to the storage tank after collecting the microcapsules.

  According to the microcapsule manufacturing apparatus of the present invention, the flow of the continuous phase liquid in the storage tank with respect to the nozzle becomes a meandering flow in which the rotational motion and the linear motion are combined without causing the nozzle to perform a special complicated movement. The dispersed phase droplets discharged from the nozzle ride on the flow of the continuous phase, and the action of shearing force is lost.

  As a result, the dispersed phase droplets ejected from the nozzles do not coalesce (unify) and the ejected droplets do not have a smaller particle size due to the shearing force from the continuous phase. can get.

  In addition, by adopting a configuration in which the separation tank is disposed adjacent to the storage tank, it is possible to continuously produce microcapsules without preparing a large capacity storage tank. This is also important for downsizing the rotating system of the storage tank, and has the effect of making it easy to control the rotational speed with a small motor.

Front view of a microcapsule manufacturing apparatus according to the present invention Plan view of the microcapsule manufacturing equipment (A) is the figure which showed the movement in the storage tank of the dispersed phase droplet discharged from the nozzle in the state where the center of the storage tank and the turntable is eccentric, (b) is a storage tank and a turntable. The figure which showed typically the movement in the storage tank of the dispersed phase droplet discharged from the nozzle in the state where the center of a coincides The figure which shows another Example which attached the separation tank.

  In the microcapsule manufacturing apparatus according to the present invention, a shaft 2 is penetrated and supported at the center of the base 1, and the shaft 2 is rotated by a motor 3.

  A rotating table 4 is fixed to the upper end of the shaft 2, and a fixing tool 5 is provided on the rotating table 4, and a storage tank 6 for storing the continuous phase m 1 is fixed in the fixing tool 5 so as not to move. . In a fixed state, the position of the fixture 5 is determined such that the center O1 of the turntable 4 and the center O2 of the storage tank 6 are eccentric.

  In addition, an airtight tank 7 is disposed at a location away from the base 1, and a dispersed phase m 2 such as an aqueous gelatin solution is held in the tank 7. The tank 7 is supplied with gas, fats and oils such as air and nitrogen through the pipe 8 and the inside thereof is pressurized, and the internal phase is pressurized by this pressure, and the dispersed phase m2 is transferred from the nozzle 10 to the continuous phase of the storage tank 6 through the pipe 9. It is discharged into m1. A heat retaining member 11 is provided on the outer periphery of the pipe 9.

  In the above, when the motor 3 is driven and the turntable 4 is rotated, the storage tank 6 rotates around the center O1 of the turntable 4, and the continuous phase m1 in the storage tank 6 forms a vortex. As a means for forming the vortex, a stirrer and a magnetic stirrer are conceivable, but the flow field formed by using these is a bowl-shaped vortex. This bowl-like vortex is not preferable because the flow rate is greatly different between the outside and the inside, and a large shearing force acts on the droplets to make the droplets smaller particles. Further, a stirrer, a propeller, or the like used for stirring may break the microcapsule by colliding with the molded microcapsule.

  When the dispersed phase m2 is discharged from the nozzle 10 to the vortex flow of the continuous phase m1 generated by rotating the turntable 4 as described above, the discharged dispersed phase once becomes a jet flow, and then a droplet having a uniform particle diameter. Is formed.

  When the center O2 of the storage tank 6 and the center O1 of the turntable 4 coincide with each other, the droplet of the dispersed phase m2 ejected from the nozzle 10 draws a circular trajectory along the vortex. In this case, since the center O2 of the storage tank 6 and the center O1 of the turntable 4 are eccentric, the nozzle 10 is the same as moving relatively linearly even though the position is fixed with respect to the turntable 4. Then, the droplet of the dispersed phase m2 discharged from the nozzle 10 draws a wavy locus as shown in FIG.

  That is, FIG. 3 shows the trajectory of the liquid droplets ejected from the nozzles (nozzle trajectory) in the continuous phase flowing from right to left in the figure. In n seconds, one liquid droplet is formed. Refers to the interval. However, in FIG. 3, the flow of the continuous phase is represented by a straight line instead of an actual circle (vortex) for easy understanding.

  When the center O2 of the storage tank 6 and the center O1 of the turntable 4 are eccentric as in the present application, the linear movement and the left-right movement are combined and a wavy locus as shown in FIG. become. As a result, the interval between the droplets increases. On the other hand, when the center O2 of the storage tank 6 and the center O1 of the turntable 4 coincide with each other, the trajectory of the droplets becomes a straight line, and the interval between the droplets becomes narrow and it becomes easy to combine them.

  In this way, the droplets of the dispersed phase m2 are discharged into the continuous phase m1 so as to draw a wavy trajectory, so that the interval between adjacent droplets is widened, making it difficult for the droplets to coalesce. Since it flows without countering the flow of m1, it does not receive a shearing force and the droplet does not become small. Therefore, the microcapsules having a uniform particle size are continuously produced without being united or miniaturized until the gelatin is gelled.

  FIG. 4 is a diagram showing another embodiment in which a separation tank is provided. In this embodiment, a microcapsule in which a separation tank 12 is arranged adjacent to a storage tank 6 and the dispersed phase m2 is gelled through a tube 13 is shown. The contained continuous phase m1 is taken into the separation tank 12 by a pump or the like (for example, a reciprocating pump or an axial flow pump is suitable for transferring the microcapsules) arranged in the middle or at the end of the tubes 13 and 14, and the microcapsules are separated. Only the recovered continuous phase m1 is returned to the storage tank 6.

  By setting it as said structure, a large quantity of microcapsules can be continuously produced, without enlarging the volume of the storage tank 6. FIG.

  Since the microcapsule manufacturing apparatus according to the present invention uses an interface between liquids that do not mix with each other, it can be applied to an interfacial polymerization method, an in-situ polymerization method, a coacervation method, a submerged drying method, and the like. can do.

  DESCRIPTION OF SYMBOLS 1 ... Base, 2 ... Shaft, 3 ... Motor, 4 ... Turntable, 5 ... Fixing tool, 6 ... Storage tank, 7 ... Tank, 8, 9 ... Piping, 10 ... Nozzle, 11 ... Thermal insulation member, 12 ... Separation tank , 13, 14 ... tube, m1 ... continuous phase, m2 ... dispersed phase, O1 ... center of rotating table, O2 ... center of storage tank.

Claims (2)

  In a microcapsule manufacturing apparatus that discharges a dispersed phase solution from a nozzle into a liquid that is a continuous phase in a storage tank, the storage tank is in a state where the rotation center of the turntable and the center of the storage tank are eccentric on the turntable. An apparatus for producing microcapsules, which is placed.   2. The microcapsule manufacturing apparatus according to claim 1, wherein a separation tank is disposed adjacent to the storage tank, and a continuous phase liquid containing the microcapsules in the storage tank is taken into the separation tank, and the microcapsules are microscopically separated in the separation tank. An apparatus for producing a microcapsule, wherein the continuous phase liquid is returned to a storage tank after the capsule is recovered.

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