JP2005186026A - Device and method of preparing emulsion - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To eliminate troublesome labor in preparation, handling and difficult operation of an emulsion device and to easily perform an emulsion preparation in a place where an emulsion device is not installed, for example, in a general household also. <P>SOLUTION: Connectors 2 connectable to a disposable syringe 6 or 7 are matched, a disk-like Shirasu-porous glass membrane porous body 1 is sandwiched between them to prepare the emulsion preparation device 3. When an emulsification working is performed, the syringe 6 or 7 in which a dispersed phase liquid or a continuous phase liquid is sampled is connected to each of the connectors 2 to alternately push a plunger 6a or 7a, thereby mixing the dispersed phase liquid and the continuous phase liquid while they are interacting with each other through the porous body, to produce the emulsified liquid of equal particle diameters. <P>COPYRIGHT: (C)2005,JPO&NCIPI

Description

  The present invention relates to an emulsifying apparatus, and more particularly to a pumping type emulsifying device capable of easily preparing an emulsified emulsion having a uniform particle diameter even in a small amount.

  Conventionally, as an emulsifying device used for emulsion preparation, a rotating body is provided in an emulsion forming chamber having a continuous phase, and the liquid in the dispersed phase liquid chamber is put into the liquid while stirring the continuous phase liquid by the rotating body, and the piston, etc. There are some which generate an emulsion by press-fitting and dispersing with a mechanical pressurizing apparatus (for example, see Patent Document 1).

Japanese Patent Laid-Open No. 06-315617

  However, in these emulsification apparatuses and emulsification methods, for example, even if the emulsification amount is a small amount of 1 ml to 100 ml, a mechanical pressurizing means is required for press-fitting the dispersed phase. Further, a rotating body power unit for stirring the liquid in the continuous phase is required, and a large incidental unit is also required for producing a very small amount of emulsion.

  In particular, simple emulsification is required, such as composition verification and particle size verification of a small amount of emulsion, but frequent repeated experiments are required, or the amount of emulsified emulsion used at one time is extremely small, and loss volume is minimized. For expensive compositions to be reduced, it is not appropriate at all, without taking into account the experimental preparation time.

  Therefore, the emulsion preparation device of the present invention is characterized in that a porous body is provided in a conduit portion formed so that a pump-type container can communicate. The second feature is that a porous body is provided in a conduit portion formed so that a pump-type container can be connected to one side and a stationary container can be connected to the other side. Further, the third feature is that the pump-type container is a syringe for injection. Furthermore, a pressure head having a nozzle and a liquid storage container in which a conduit for pumping liquid is inserted and a premixed mixture of a dispersed phase liquid and a continuous phase liquid are stored. The fourth feature is that the emulsified emulsion is generated and discharged from the nozzle through the porous body by applying pressure to the nozzle. That is, an emulsion is generated by reciprocating a dispersed phase or a continuous phase or an emulsion in which a dispersed phase and a continuous phase are mixed in advance between at least two chambers partitioned through a porous body. An emulsion preparation method is provided.

  For example, in the present invention, particle diameters are uniformed by using a syringe (for example, a commercially available syringe that is easily available) that matches the preparation amount of the emulsion, without providing a dispersed phase chamber and a continuous phase chamber. An emulsion can be prepared. Therefore, the emulsion can be easily prepared in the palm without requiring special equipment for the emulsification operation.

  In addition, if you want to prepare in a sterile condition like a chemical solution, collect the dispersed phase and continuous phase with a sterilized syringe, respectively, and collect the sterilized with a porous body in the conduit that connects the pair of syringes. By connecting the continuous phase liquid and the dispersed phase liquid alternately through the porous body, the emulsion emulsion having gradually uniform particle diameters can be generated.

  In addition, a mixture of a dispersed phase and a continuous phase is collected with one syringe in advance and press-fitted into the other syringe, or directly into a container to produce an emulsion having a uniform particle size. Things are also possible. There are O / W type emulsions and W / O type emulsions in the form of emulsified emulsions. If the surface of the porous body is subjected to a hydrophilic treatment or a hydrophobic treatment depending on the form of the emulsion, O / W type emulsions are provided. W-based and W / O-based emulsions can be produced. As a result, composite emulsions such as W / O, O / W, O / W / O / W, and W / O / W / O types can be easily prepared in the palm without requiring a large-scale apparatus. Can do

  The present invention relates to preparation of an emulsifying device, such as the difficulty of preparing an emulsion in a sterile state as a sterilized disposable device, and the troublesomeness of washing, drying, assembly and sterilization of the emulsifying device in repeated verification experiments. The emulsifier is not only the need for large-scale emulsifiers and incidental devices, but also the preparation time of these devices is not required at all. Can be easily prepared even in a place where is not installed, for example, in a general household.

DESCRIPTION OF THE PREFERRED EMBODIMENTS Embodiments of the present invention will be described below based on examples shown in the drawings. Needless to say, the present invention is not limited to the contents of the following examples and descriptions.
FIG. 1 is an exploded perspective view of an emulsion preparation device according to the present invention, FIG. 2 is a perspective view showing a state where the emulsion preparation device according to the present invention of FIG. 1 is assembled, and FIG. 3 shows a disc-shaped thin film porous body. 4 is a perspective view showing a tube bundle-shaped porous body, FIG. 5 is a perspective view showing a state in which a pair of syringes are connected to both ends of the device according to the present invention, and FIG. 6 is a syringe in one of the devices according to the present invention. And FIG. 7 is a perspective view showing another use state of the device according to the present invention.

  As shown in FIG. 1 to FIG. 5, the emulsion preparation device 3 according to the present example is made by connecting connectors 2 that can be connected to a disposable syringe 6 or 7 described later, with a disc-shaped shirasu porous glass film therebetween. The porous body 1 is sandwiched between them. That is, when emulsifying work is performed, the syringe 6 or 7 that collects the dispersed phase liquid or the continuous phase liquid is connected to the end of each connector 2 and the plungers 6a or 7a are alternately pushed. The dispersed phase liquid and the continuous phase liquid can be mixed while being exchanged through the porous body to produce an emulsion having a uniform particle size.

  In addition, examples of the porous body in the present invention include a metal porous body, a glass porous body, a wooden porous body, and a plated porous body. In the present invention, the porous body has a uniform pore diameter. An inorganic porous body having a high porosity is preferable.

  In addition, as shown in FIG. 6, a disposable syringe 8 obtained by collecting a premix of a dispersed phase liquid and a continuous phase liquid may be attached to one of the devices 3, and a stationary extraction container 9 may be attached to the other. As shown in FIG. 7, in a pump-type container composed of a pressure head 11 having a nozzle 13 and a liquid storage container 10 having a liquid pumping pipe 12 inserted therein, a preliminary dispersion of a dispersed phase liquid and a continuous phase liquid is provided. An emulsion may be produced and poured out from the nozzle 13 through the porous body 14 by putting a mixture and applying pressure in a pumping manner.

(Experimental example 1)
Shirasu porous glass (hereinafter referred to as SPG) having a uniform pore diameter and a high porosity in a range of 0.05 μm to 20 μm was used as the inorganic porous membrane for the porous body. SPG is one of the preferred porous bodies used in the present invention. The porous body 1 used for the device for preparing an O / W emulsion is subjected to a hydrophilization surface treatment with a hydrophilizing solution that easily wets in continuous phase water, and is used for a device for preparing a W / O emulsion. The porous body 1 can be subjected to a hydrophobized surface treatment with a hydrophobizing solution that easily wets in continuous phase oil.

As shown in FIG. 5, the SPG film as the porous body 1 is a disk-shaped one having an outer diameter of 6.5 mm and a thickness of 0.8 mm, and the connector 3 is excellent on the premise of mass production as a general medical device. Disposable pumping devices (see Fig. 1) were manufactured using inexpensive vinyl chloride resin molded parts that had excellent moldability and solvent adhesion. The dispersed phase liquid is collected in the syringe 6 and the continuous phase liquid is collected in the syringe 7, connected to both ends of the pumping device 3, and an O / W emulsion emulsion is generated by a pumping operation in which the syringe plungers 6 a and 7 a are alternately pushed. did. Table 2 shows the relationship between the SPG membrane pore size, the number of pumping times, and the emulsion emulsion particle size, and FIG. 8 shows the relationship diagram.

(Experimental example 2)
Table 2 shows the time required to produce an emulsion particle size of about 2 μm by the pumping membrane emulsification according to the present invention and the conventional direct membrane emulsification. As can be seen from Table 2, in direct membrane emulsification, the emulsified emulsion particle size swells to about 3 to 3.5 times the SPG membrane pore size, so that the desired particle size can be obtained. The emulsified membrane used in the invention needs to have a pore size smaller than the particle size of the emulsified emulsion. For this reason, it is necessary to reduce the amount of pressurization required to obtain an emulsion having a uniform particle size. Therefore, the emulsification rate is very slow and the emulsion generation time tends to be long. However, according to the pumping membrane emulsification by the device of the present invention, since the emulsion emulsion particle size can be reduced only by repeating the pumping several times, the SPG membrane pore size larger than the emulsion emulsion particle size of the desired size is used. In addition, an emulsified emulsion can be produced in a much shorter time than direct membrane emulsification.

(Experimental example 3)
As shown in FIG. 7, in a pump-type container composed of a pressure head 11 having a nozzle 13 and a liquid storage container 10 having a liquid pumping pipe 12 inserted therein, a preliminary dispersion of a dispersed phase liquid and a continuous phase liquid is provided. An emulsified emulsion was produced by a pump-type hand spray in which the mixture was placed and pressure was applied in a pumping manner to produce and dispense the emulsified emulsion from the nozzle 13 through the porous body 14.
As the porous body 14 at this time, a cylindrical tubular SPG film having an outer diameter of 10 mm, an inner diameter of 8.5 mm, and a length of 20 mm and having a pore diameter of 3 μm was used. The dispersed phase liquid and the continuous phase liquid were put into the liquid storage container 10, and the container 10 was shaken to pre-emulsify. Thereafter, the pressing head 11 was pumped several times and filtered and emulsified through the porous body 14 to produce and dispense an emulsified emulsion having a uniform particle diameter from the nozzle 13 outlet.

  FIG. 9 shows the emulsion particle diameter finally obtained by the pump-type hand spray, the emulsion particle diameter preliminarily emulsified in the liquid storage container 10, and the pumping conduit portion 12 does not include the porous body 14. It is a distribution map of the emulsion particle diameter discharged from the nozzle 13 using a spray. Here, the distribution L1 indicates a coarse emulsion particle size distribution when the dispersed phase liquid and the continuous phase liquid are put into the liquid storage container 10 and shaken manually to pre-emulsify. The distribution L2 indicates the emulsion particle size distribution in which the pre-emulsified emulsion is pumped only by a tube without providing the porous body 14 in the pumping conduit section 12 and is discharged from the nozzle 13. The distribution L3 shows the emulsion particle size distribution in which a porous body 14 (SPG film) is provided at the tip of the pumping conduit section 12 and a coarse emulsion preliminarily emulsified is further discharged from the nozzle 13 through the porous body 14.

  As is apparent from this particle distribution state, the emulsion particle size distribution L1 pre-emulsified in the liquid container has a particle size distribution spread of about 2 μm to 500 μm, and the emulsion particle size is not uniform. The distribution L2 is reduced by the spray action of the nozzle 13, but it is difficult to say that it is uniform due to the emulsion particle size distribution of about 1 μm to 100 μm. That is, by providing the SPG film 14 in the conduit portion, an emulsified emulsion having a uniform emulsion particle diameter of about 1 μm to 9 μm can be generated as in the distribution L3.

  The present invention makes it possible to prepare an emulsion aseptically as a sterilized disposable device. When developing new drugs for emulsion formulations such as DDS therapy in the medical field, it is easy to encapsulate various chemical solutions such as animal experiments. In addition, it is possible to prepare a prototype and make a prototype, and it is possible to easily carry out repeated experiments. In addition, it is easy to prepare emulsion capsule flavors for foods with regular grains even in general households. For bakery foods with flavors such as bakery stores, originals such as those that only need about 10 ml per 1 kg of dough per day are sold. A bakery food with capsule flavor that is rich in properties can be easily produced. In addition, it is possible to spray and spread by agrochemicals or aquaculture while encapsulating active ingredients in the process of spraying volatile chemicals and fertilizers. Thus, since the present invention can easily prepare emulsions with uniform particle diameters in a short time, it is very useful for developing emulsion technology, and is a practical and innovative device for preparing emulsions. As for the pump-type device as shown in FIG. 7, there is an electrolyzed water generating device that modifies the water cluster to a small size, but without requiring such a large and expensive device, a handy type pumping is possible. By using a porous body having small pores in an expression device, it is possible to produce reformed water that is inexpensive and has a small water cluster.

It is a disassembled perspective view of the device for emulsion preparation which concerns on this invention. It is a perspective view which shows the state which assembled the device for emulsion preparation which concerns on this invention. It is a perspective view which shows a disk shaped thin film porous body. It is a perspective view which shows a tube bundle-shaped porous body. It is a perspective view which shows the state which connected a pair of syringe to the both ends of the device which concerns on this invention. It is a perspective view which shows the state which attached the syringe to one side of the device which concerns on this invention, and the stationary container to the other. It is a perspective view which shows the other use condition of the device which concerns on this invention. It is a graph which shows the frequency | count of pumping of a hand pump type device, and an emulsion emulsion particle diameter. It is the distribution map which compared the emulsion particle diameter.

Explanation of symbols

DESCRIPTION OF SYMBOLS 1 Porous body 2 Connector 3 Emulsion preparation device 4 Thin-film porous body 5 Tube bundle body 6 Liquid-filled syringe 6a Plunger 7 Liquid-filled syringe 7a Plunger 8 Liquid-filled syringe 8a Plunger 9 Emulsion emulsion extraction container (stationary container)
DESCRIPTION OF SYMBOLS 10 Liquid container 11 Press head 12 Liquid pumping conduit 13 Nozzle 14 Cylindrical porous

Claims (5)

A device for preparing an emulsion, characterized in that a porous body is provided in a conduit portion formed so that a pump-type container can communicate therewith. A device for preparing an emulsion, characterized in that a porous body is provided in a conduit portion formed so that a pump-type container on one side and a stationary container on the other side can be connected. The emulsion preparation device according to claim 1 or 2, wherein the pump-type container is a syringe for injection. A pressure head having a nozzle, and a liquid storage container in which a pre-mixture of a dispersed phase liquid and a continuous phase liquid is stored, and a pressure pumping type pressure is applied to the pressure head. An emulsion preparation device characterized in that an emulsion emulsion is generated and discharged from a nozzle through a porous body by addition. An emulsion characterized in that an emulsion is produced by reciprocating a dispersed phase or a continuous phase or an emulsion in which a dispersed phase and a continuous phase are preliminarily mixed between at least two chambers partitioned through a porous body. Preparation method.

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