JP2007313466A - Emulsifying apparatus - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide an emulsifying apparatus having a simple structure and yet capable of preparing an emulsion having a fine and uniform particle size. <P>SOLUTION: An emulsifier 10 comprises a continuous-phase supply piping system, a dispersed-phase supply piping system, and an emulsion discharge piping system each in communication with the emulsifier 10 which is equipped with a continuous-phase introduction path 11 for preparing a primary emulsion by ejection of a dispersed-phase into a continuous-phase flowing in the continuous-phase introduction path 11 in communication with the continuous-phase supply piping system from a nozzle disposed in a dispersed-phase introduction path 12 in communication with the dispersed-phase supply piping system, an agitation chamber 14 for agitating the primary emulsion disposed downstream of and adjacent to the continuous-phase introduction path 11, a flow path 15 for preparing a secondary emulsion by further micronizing the primary emulsion disposed downstream of and adjacent to the agitation chamber 14, and a deceleration chamber 16 disposed downstream of and adjacent to the above flow path 15 for decelerating the secondary emulsion and transferring the same to the emulsion discharge piping system. <P>COPYRIGHT: (C)2008,JPO&INPIT

Description

  The present invention relates to an emulsifying apparatus for producing an emulsion in which a dispersed phase such as oil or water is uniformly dispersed in a continuous phase such as water or oil.

Emulsion is the addition of a surfactant (emulsifier) to two liquids that do not mix with each other, such as water and oil, and operations such as stirring are performed to make the oil droplets uniform in water (or water droplets in oil). Dispersed liquid-liquid emulsion.

  As a conventional general emulsion production method, batch production is known. This is a production method in which a raw material for a continuous phase or a dispersed phase and a surfactant are introduced into a large container and a large amount of emulsion is produced at once using a rotating / stirring mechanism. However, there are several problems with this production method.

  The first is that the droplet size is not uniform and has a distribution. The reason is that the shearing force applied during rotation and stirring is not uniformly applied to the entire liquid. And in order to stabilize this particle size distribution to a fixed value, rotation and stirring for 20 minutes or more are required, and it takes time.

  In the state where the particle size of the emulsion is not uniform, the effect and performance vary and cause quality degradation.

  The second problem is that the equipment becomes larger. Batch production requires a variety of mechanisms, such as a mechanism for feeding liquid into a container, a mechanism for stirring liquid, and a mechanism for taking out liquid from the container, which makes the apparatus large and requires time and labor for adjustment and cleaning of the apparatus. .

  As a production (emulsification) device that solves the above problem, as disclosed in Patent Document 1 below, a plurality of plate bodies provided with a plurality of holes are stacked in multiple stages at regular intervals, 2. Description of the Related Art A flow pipe type emulsifying device is known in which an emulsion having a fine particle size is obtained by an action such as liquid collision by repeatedly causing merging.

JP 2003-260343 A

  The flow tube type emulsifying device of the above prior art sends the continuous phase and the dispersed phase into the tube and repeats the diversion / merging to continuously produce the emulsion, but the two phases are fed in a non-uniformly mixed state. In this case, in order to produce an emulsion having a particle size of about several μm, it is necessary to repeat the diversion and merging many times. Therefore, the plates are laminated in multiple stages, the equipment is complicated, and it takes time to manufacture the equipment. It takes.

  In addition, when the non-uniformity is large, the emulsion particle size may vary even if the diversion and merging are repeated.

  Therefore, an object of the present invention is to provide an emulsifying apparatus capable of producing an emulsion having a fine and uniform particle diameter even with a simple configuration.

  The emulsifying apparatus of the present invention that achieves the above object is characterized by an emulsifier that produces an emulsion in an emulsifying apparatus that produces an emulsion in which a dispersed phase such as oil or water is uniformly dispersed in a continuous phase such as water or oil. A continuous phase supply piping system for supplying a continuous phase to the emulsifier, a dispersed phase supply piping system for supplying a dispersed phase to the emulsifier, and an emulsion discharge for discharging the emulsion produced by the emulsifier from the emulsifier The emulsifier discharges a dispersed phase from a nozzle provided in a dispersed phase introduction path communicating with the dispersed phase supply piping system into a continuous phase flowing in a path communicating with the continuous phase supply piping system. A continuous phase introduction path for producing a primary emulsion, a stirring chamber adjacent to the continuous phase introduction path downstream thereof and stirring the primary emulsion, and adjacent to the stirring chamber downstream thereof and the primary emulsion A flow path for producing a secondary emulsion by refining the flow path, and a speed reducing chamber that is adjacent to the flow path on the downstream side and decelerates the secondary emulsion and sends it to the emulsion discharge piping system. It is in.

  According to the apparatus of the present invention, a primary emulsion having a uniform dispersed phase size is produced in the continuous phase introduction path, and the dispersed phase is uniformly diffused into the continuous phase by stirring in the stirring chamber. Since it is sheared and refined, an emulsion having a fine and uniform particle size can be produced even with a simple configuration.

  Hereinafter, embodiments shown in the drawings will be described.

  In FIG. 1, the system configuration | structure of the emulsification apparatus 1 which becomes one Embodiment of this invention is shown. In this example, an O / W (oil in water) type emulsion in which oil droplets are dispersed in water using a mixture of water and a surfactant as a continuous phase and edible oil as a dispersed phase is produced. deal with.

In FIG. 1, the continuous phase that becomes the solvent of the emulsion and the dispersed phase that becomes the solute are stored in separate liquid tanks 91A and 91B. The liquids (continuous phase and dispersed phase) stored in the liquid tanks 91A and 91B are respectively supplied with liquid supply tubes 92A and 92B, pumps 93A and 93B installed in the middle thereof, and check valves 94A and 94B for preventing backflow. Filter 95A for removing foreign matter,
After passing through 95B, the liquid is fed to a small rectangular emulsifier 10 having a length and width of about 10 mm square and a length of about 40 mm. The piping system connected to the liquid feeding tube 92A is a continuous phase supply piping system, and the piping system connected to the liquid feeding tube 92B is a dispersed phase supply piping system.

  As the liquid feeding tubes 92A and 92B, it is preferable to use a fluororesin tube or the like which has high corrosion resistance and is hard and hard to expand.

  The pumps 93A and 93B use a syringe pump with excellent liquid feeding accuracy or a diaphragm pump capable of intermittent liquid feeding when the liquid feeding conditions are frequently changed, such as for experimental purposes. When continuous liquid feeding is required, it is preferable to use a gear pump or a rotary pump.

  For these pumps 93A and 93B, a low-pressure pump having a discharge pressure of about several atmospheres is sufficient for the reason described later, and a syringe pump is used in this embodiment.

  The emulsifier 10 is provided with a temperature adjusting mechanism (temperature adjusting mechanism) 96 for adjusting the liquid viscosity and stabilizing the emulsion particle diameter, and is adjusted to a temperature for controlling an arbitrary emulsification temperature.

  The temperature control mechanism 96 desirably has both heating and cooling functions in order to cope with various conditions. In this embodiment, a Peltier element that can be heated and cooled by controlling the direction of current is provided in the plate. And the emulsifier 10 was installed on the plate. The temperature adjusting means may be a thermostatic bath or a hot water bath. As these temperature control mechanisms 96, since the emulsifier 10 is small, a small thing with low energy consumption is sufficient.

The emulsion produced by the emulsifier 10 is stored in an emulsion tank 98 through a liquid feed tube 97 made of the same material as the liquid feed tubes 92A and 92B.
Hereinafter, the configuration of the emulsifier 10 will be described in detail.
FIG. 2 is a perspective sectional view of the emulsifier 10.

  In the present embodiment, the material of the emulsifier 10 is not particularly limited, and materials such as metal, glass, silicon, and resin are appropriately selected according to the type of liquid to be fed. Further, the machining method may be a one-piece machined part, and as long as liquid leakage does not occur, the parts that are divided and processed may be assembled by bonding, welding, fastening with screws, or the like.

  The emulsifier 10 has a continuous phase introduction path 11 that communicates with a liquid feeding tube 92A of a continuous phase supply piping system and a dispersed phase introduction path 12 that communicates with a liquid feeding tube 92B of a dispersed phase supply piping system. The continuous phase introduction path 11 extends in the longitudinal direction of the emulsifier 10, and the dispersed phase introduction path 12 is provided so as to be orthogonal to the continuous phase introduction path 11.

  The nozzle 13 is provided in the dispersed phase introduction path 12, and the primary emulsion is produced in the continuous phase introduction path 11 by discharging the dispersed phase from the nozzle 13 to the continuous phase flowing in the continuous phase introduction path 11.

  A stirring chamber 14 for stirring the primary emulsion is adjacent to the downstream side of the continuous phase introduction path 11, and a flow path 15 for producing a secondary emulsion by refining the primary emulsion is adjacent to the downstream side of the stirring chamber 14. The speed reducing chamber 16 for decelerating the secondary emulsion and sending the emulsion to the liquid feeding tube 97 of the emulsion discharge piping system is adjacent to the downstream side of the emulsion discharging pipe system. Communicate.

  The continuous phase introduction path 11 is a cylindrical flow path having a diameter of several millimeters, and is connected to the liquid feeding tube 92A by a threaded portion and a connection joint (not shown), and the continuous phase flows in the direction of arrow A in the figure. The dispersed phase introduction path 12 is also a cylindrical channel having a diameter of several millimeters, and is connected to the liquid feeding tube 92B by a screw portion and a connection joint (not shown), and the dispersed phase flows in the direction of arrow B in the figure.

  The nozzle 13 is provided at an end portion of the dispersed phase introduction path 12 which is a merging portion of the continuous phase introduction path 11 and the dispersed phase introduction path 12, and the dispersed phase is discharged from the nozzle 13 so that the particle diameter is uniform (equal). ) A fine primary emulsion is obtained.

  FIG. 3 is a perspective sectional view of the continuous phase introduction path 11 in the emulsifier 10, and shows the nozzle 13 in an enlarged manner.

  The nozzle 13 is a cylindrical part made of a separate part from the emulsifier 10 and having a slightly smaller outer diameter than the dispersed phase introduction path 12, and has a number of minute through holes 19 in the length direction. Further, the downstream side of each opening 19 is open to the head of the (cutting) conical protrusion (projection) 20.

  The protrusion 20 is formed by cutting the surface of the nozzle 13 with an extremely fine end mill. Since the angle of the protrusion 20 is adjusted to the tip angle of the edge of the end mill, the protrusion 20 can be easily formed on the nozzle 13 simply by cutting the end mill so as to draw a circle, and the productivity is excellent.

  The nozzle 13 is inserted into the dispersed phase introduction path 12 and fixed in contact with a ring-shaped nozzle support surface 18 provided with a reduced flow path diameter at the tip of the dispersed phase introduction path 12. The fixing method may be any method such as adhesion, press-fitting, or pressing with a connecting joint. In this embodiment, the nozzle 13 is a separate part for easy processing, but it may be processed integrally with the emulsifier 10.

  The dispersed phase flowing in the direction of arrow b through the dispersed phase introduction path 12 is divided into 17 circular openings 19 formed in a circle, passes through the protrusions 20 at the tip, and passes through the continuous phase introduction path 11 in the direction of arrow a. It is discharged and sheared into the flow of the continuous phase flowing in a form orthogonal to the droplets to form a dispersed phase of droplets.

  The particle size of the droplets can be adjusted by changing the flow rate ratio between the continuous phase and the dispersed phase. Further, by providing the protrusions 20 on the inner side of the continuous phase introduction path 11, the dispersed phase is more easily sheared than in the case of merely providing holes on the plane, and the uniformity of the particle diameter is improved.

  Since the size of the primary emulsion is not a problem as long as the dispersed phase has the same particle size, the diameter of the opening 19 is set to 0.2 mm in consideration of pressure loss and the like in this embodiment. This is larger than the conventionally known microchip channel dimensions. By increasing the size of the flow path in this way, the increase in pressure loss is suppressed, and in the case of a liquid with low viscosity, the pressure loss is suppressed to tens of kPa or less even if the liquid amount is about several tens to 100 ml / min. It becomes possible.

  In this embodiment, the dispersed phase is continuously fed using a syringe pump, but may be delivered intermittently using a diaphragm pump or the like. By performing intermittent liquid feeding, liquid discontinuity of the dispersed phase at the micro nozzle part can be improved, and the droplet diameter can be made more uniform.

  This makes it possible to more effectively reduce the size of the emulsion in the flow path 15 described later. In addition, the emulsion concentration can be controlled by adjusting the cycle of intermittent liquid feeding.

  FIG. 4 is a view for explaining the state of emulsion production in the emulsifier 10, and shows a longitudinal section of the emulsifier 10.

  As shown in FIG. 4, the stirring chamber 14 has a cylindrical shape with a larger diameter than the continuous phase introduction path 11 and the flow path (throttle section) 15. As will be described later, the diameter of the throttle portion (flow path) 15 is extremely smaller than that of the continuous phase introduction path 11 in order to realize a high flow rate, and therefore, most of the primary emulsion sent from the continuous phase introduction path 11 is Immediately, it does not pass through the constricted portion 15 and becomes a swirling flow circulating in the stirring chamber 14 having a large space as indicated by an arrow C in the figure, where the continuous phase and the dispersed phase become more uniform by swirling. Is stirred as such.

The tip on the downstream side of the stirring chamber 14 (the area following the flow path (throttle portion) 15 of the stirring chamber 14) has a conical shape (conical shape) that narrows toward the throttling portion 15 and smoothly rotates the primary emulsion. There is an effect to do. Since the angle of the cone is matched to the tip angle of the machining drill, machining can be performed easily.

  The primary emulsion in which the dispersed phase having a uniform particle diameter after the above-described process is uniformly dispersed in the continuous phase passes through the squeezed portion 15, whereby the dispersed phase is refined and becomes a secondary emulsion having a minute particle diameter. .

  The throttle portion (flow channel) 15 has a cylindrical shape with a small diameter and a short length, and the primary emulsion flowing therethrough is rapidly accelerated by a decrease in the cross-sectional area of the flow channel, resulting in shearing force from the wall surface. Is instantaneously miniaturized.

  If there is a variation in the continuous phase and the dispersed phase that pass through the squeezed portion 15, the particle size of the secondary emulsion after refinement also varies, but the primary emulsion has a uniform particle size and is uniformly dispersed. A fine secondary emulsion having a uniform particle diameter can be obtained by passing the squeezed portion 15 once.

  Since the refinement at the narrowed portion 15 is more conspicuous as the flow velocity is larger, it is desirable to increase the flow rate of the primary emulsion or to reduce the diameter of the narrowed portion 15 when producing a fine secondary emulsion. .

In this embodiment, the throttle portion 15 has a diameter of 0.3 mm and a length of 1 mm.
A fine secondary emulsion having a diameter of several μm was obtained at about min. Moreover, the increase in pressure loss was suppressed by setting the length to 1 mm, and when a low viscosity oil was used, even when a flow rate of 100 ml / min was fed, only a pressure loss of 0.5 MPa or less occurred. .

  Since drilling with a diameter of 0.1 mm can be performed relatively easily, when the diameter of the throttle portion 15 is 0.1 mm, the primary flow rate is about 10 ml / min from the result of this embodiment. Emulsion can be refined at low pressure.

  In this embodiment, the drawn portion 15 has a simple cylindrical shape for ease of processing. However, the shape of the drawn portion 15 may be triangular, if the particle size is uniform and sufficient shear force can be applied to the uniformly dispersed primary emulsion. It may be a polygon such as a rectangle or a hexagon.

  The deceleration chamber 16 is a portion connecting the throttle portion 15 and the emulsion discharge passage 17 and has a larger cylindrical shape than the throttle portion 15 and the emulsion discharge passage 17 in order to reduce pressure loss.

  The emulsion discharge path 17 is a cylindrical flow path having a diameter of 3 mm, and is connected to the liquid feeding tube 97 by a connection joint (not shown). The secondary emulsion flows in the direction of the arrow D in the figure and is discharged out of the emulsifier 10. .

  As described above, according to the apparatus of the present invention, a secondary emulsion having a uniform and fine particle size can be obtained by producing a primary emulsion in which the dispersed phase has a uniform particle size and is uniformly dispersed in a continuous phase. Can be obtained. As the dispersed phase becomes finer, the binding force acting between the dispersed phases becomes weaker, and the separation of the dispersed phase and the continuous phase with the passage of time and deterioration of the emulsion are reduced, and high quality can be maintained.

  The configuration of the emulsifying device 1 is simple, the emulsifier 10 is simple to process each part and easy to produce, and because of the structure in which all parts are integrated, there are no extra joints or pipes between the parts. The emulsion does not change therein, and the uniformity of the emulsion particle size can be further improved.

  In addition, it is possible to continuously produce an emulsion simply by feeding a liquid with the pumps 93A and 93B, and it is not necessary to separately provide a liquid dispensing mechanism and a stirring mechanism as in batch production. Can be miniaturized and simplified.

In the embodiment shown in FIGS. 1 to 4, the dispersed phase introduction path 12 is provided only on one surface side of the emulsifier 10 having a square cross section, but the other side is orthogonal to the opposing surface or both surfaces. In addition, the disperse phase can be supplied (discharged) more evenly from the periphery of the continuous phase flowing through the continuous phase introduction path 11 via the nozzles having a plurality of holes. it can. If the cross section of the emulsifier 10 is substantially triangular or hexagonal, the dispersed phase is supplied more evenly from three or six directions to the continuous phase of the continuous phase introduction path 11 through a nozzle having a plurality of holes. (Discharge) can also be performed.

  In FIG. 2, the dispersed phase introduction path 12 is installed so as to be orthogonal to the continuous phase introduction path 11, but the dispersed phase discharged from the nozzle 13 is in the direction of the arrow a in the figure in the continuous phase introduction path 11. A disperse phase introduction path 12 having an inclination angle with respect to the continuous phase introduction path 11 is installed so as to go backward with respect to the continuous phase flow, or along the continuous phase flow in the direction of the arrow a. Alternatively, a disperse phase introduction path 12 having an inclination angle with respect to the continuous phase introduction path 11 may be installed.

  When the dispersed phase introduction path 12 is installed with an inclination angle that goes back to the flow of the continuous phase, the dispersed phase discharged from the nozzle 13 is a continuous phase flow that is easily cut off, and the particle size of the dispersed phase in the primary emulsion is uniform. In addition to becoming, the mixing effect is also high. Further, when the dispersed phase introduction path 12 having an inclination angle is installed so as to follow the flow of the continuous phase, the dispersed phase can be smoothly joined to the flow of the continuous phase, so the pressure loss does not increase, and the pump 93B Can save energy.

  Further, the nozzle 13 may be annular, and the openings 19 may be provided in the radial direction on the entire circumference so as to supply (discharge) the dispersed phase more evenly.

In these cases, since the amount of supply (discharge) of the dispersed phase is large, the flow rate of the pump 93B is lowered or the dispersed phase is sucked at the flow rate of the continuous phase flowing through the continuous phase introduction path 11 to Can be omitted by providing a flow rate adjusting valve in the dispersed phase supply piping system and adjusting the opening of the valve.

  FIG. 5 is a system configuration diagram showing a different embodiment of the present invention.

  When performing multi-product small-quantity production, it is preferable that a plurality of products can be produced with the same apparatus, and it is desirable that the production amount can be easily increased or decreased.

Therefore, in the embodiment shown in FIG. 5, a plurality of emulsifiers 10a to 10c are installed in parallel, and a plurality of liquid tanks 91a to 91n are installed to store the raw materials, and different raw materials are stored. These emulsifiers 10a to 10c and liquid tanks 91a to 91n are connected as shown in the figure via switching valves (raw material side valves 81a to 81c, 82a to 82c, emulsifier side valves 85a to 85c, 86a to 86c). To do.

By switching the raw material side valves 81a to 81c and 82a to 82c, the pump 93A,
The type of liquid fed from 93B can be changed, and a plurality of products can be produced.

  Moreover, the number of the emulsifiers 10 used for a process can be adjusted by switching the emulsifier side valve | bulb 85a-85c, 86a-86c. If the discharge amount from the pumps 93A and 93B is increased and the number of emulsifiers to be used is increased, the same emulsion as when one emulsifier is used can be produced in large quantities in proportion to the number.

  When using a metering pump, the flow rate per unit can be adjusted by increasing or decreasing the number of emulsifiers, and the particle size of the emulsion can be adjusted without changing the operation of the pumps 93A and 93B. It becomes possible to do.

  In FIG. 5, the check valve and the filter shown in FIG. 1 are omitted, but they may be installed, and the temperature control mechanism 96 may be installed individually for each of the emulsifiers 10a to 10c.

It is a system configuration figure showing one embodiment of the present invention. It is a perspective sectional view of the emulsifier in FIG. FIG. 3 is a perspective sectional view of the continuous phase introduction path of the emulsifier in FIG. 2. It is a figure explaining the condition of emulsion production with the emulsifier in FIG. It is a system configuration figure showing a different embodiment of the present invention.

Explanation of symbols

DESCRIPTION OF SYMBOLS 1 ... Emulsification apparatus, 10 ... Emulsifier, 11 ... Continuous phase introduction path, 12 ... Dispersed phase introduction path, 13 ... Nozzle, 14 ... Stirring chamber, 15 ... Flow path (throttle part), 16 ... Deceleration chamber.

Claims (8)

In an emulsifying apparatus for producing an emulsion in which a dispersed phase such as oil or water is uniformly dispersed in a continuous phase such as water or oil,
An emulsifier for producing an emulsion, a continuous phase supply piping system for supplying a continuous phase to the emulsifier, a dispersed phase supply piping system for supplying a dispersed phase to the emulsifier, and an emulsion produced by the emulsifier Has an emulsion discharge piping system that discharges from the vessel,
The emulsifier produces a primary emulsion by discharging a dispersed phase from a nozzle provided in a dispersed phase introduction path communicating with the dispersed phase supply piping system to a continuous phase flowing in a path communicating with the continuous phase supply piping system. The continuous phase introduction path, the stirring chamber adjoining the continuous phase introduction path downstream thereof and stirring the primary emulsion, and the secondary emulsion adjoining the stirring chamber adjacent downstream thereof and refining the primary emulsion And a decelerating chamber that is adjacent to the flow channel on the downstream side thereof, decelerates the secondary emulsion, and sends it to the emulsion discharge piping system.   The emulsifying apparatus according to claim 1, wherein the stirring chamber in the emulsifier has a larger diameter than the continuous phase introduction path, the flow path has a smaller diameter than the continuous phase introduction path, and the deceleration chamber has a larger diameter than the flow path. An emulsification apparatus characterized by the above.   2. The emulsifying apparatus according to claim 1, wherein the nozzle of the emulsifier includes a plurality of apertures through which a dispersed phase is discharged.   4. The emulsifying apparatus according to claim 3, wherein each of the openings in the nozzle opens at the top of a projecting portion that projects in a conical shape inside the continuous phase introduction path.   2. The emulsifying apparatus according to claim 1, wherein a region of the emulsifier following the flow path of the stirring chamber is conical.   2. The emulsifier according to claim 1, wherein the emulsifier includes a temperature adjusting mechanism for controlling an emulsification temperature.   The emulsifying apparatus according to claim 1, wherein the continuous phase supply piping system and the dispersed phase supply piping system each include liquid feeding means for supplying a desired amount of the continuous phase and the dispersed phase to the emulsifier. Emulsifying device. 2. The emulsifying apparatus according to claim 1, wherein the dispersed phase introduction path is installed perpendicularly to the continuous phase introduction path or with an inclination angle.

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