JP2002248328A - Emulsifying/dispersing device - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a method/device for emulsification of dispersing which performs fine particle dispersing and fine emulsification and dispersing of fine particle-containing liquid stably. SOLUTION: In the method for making a liquid or solid (a) in the mixture of the liquid or solid (a) and a liquid (b) into fine particulates to emulsify or disperse them, the method/device for emulsification or dispersing allows the mixture to pass through one or more thin hole parts having inner diameters 0.1 to 5 mm characteristically. It is preferable that the device has a resistive element preventing the flow of the mixture and having a front part in a conical shape in the rear of the thin hole parts and that the inner walls of the thin hole parts have spiral grooves and recessed or projecting resistive shapes.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an emulsifying and dispersing apparatus for dispersing fine particles, emulsifying and dispersing varnish-like substances in various industrial fields such as chemicals, paints and pigments, foods, semiconductors, and chemistry. .

[0002]

2. Description of the Related Art Conventionally, a ball mill, a homomixer, a high-speed stirring system, an ultrasonic dispersing machine, a high-pressure emulsifying dispersing machine, a high-pressure collision dispersing machine and the like have been used as emulsifying and dispersing apparatuses. In recent years, a high-speed rotating stirrer has been used for emulsifying and dispersing a varnish-like liquid, and a high-pressure collision-type dispersing apparatus has been effective for dispersing fine particles. The high-speed rotary stirrer has a high rotation speed and high rotation speed of, for example, 3000 rpm or more and a peripheral speed of 20 m / sec or more, and has a shape in which a stirring portion is devised to cause liquid / liquid shearing, shearing, and the like. I have.

[0003] The basic type of the high pressure collision type dispersion apparatus is as follows.
It is roughly divided into the following two formats. One is to form a flow path by providing a groove and a through hole in the block, and branch the flow path into two in the middle to form a thin tube (usually, the diameter is usually 100 μm or less),
It is a structure to join these again. The liquid material is caused to flow at a high speed in the flow path, and is made to collide at a junction at a high speed after being branched. Therefore, it is characteristic that the collision of the liquid material occurs in the flow path. The other is a structure having two flow paths having a larger diameter (for example, 1 mm or more) than the nozzle, and having a nozzle with a small diameter at each end. The liquid material is supplied to each of the flow paths, is ejected at a high speed from a nozzle at the tip, and collides with each other to be dispersed.

A high-speed rotary stirrer effectively performs fine emulsification and dispersion on a varnish-like liquid, and is effective in improving quality and characteristics. However, cavitation may occur, and a high-viscosity liquid may be stirred. Has limitations. On the other hand, the high-pressure collision type dispersion apparatus is a method suitable for fine particle dispersion, but depending on the structure of the apparatus, there are narrow parts of the flow path such as the nozzle part, cylindrical ejection part, chamber flow path, etc. Depending on the viscosity, the fluidity may be reduced in this portion and the fluid may not flow. Even when flowing, obstacles such as separation of the particles and the mixed solvent often appear. Further, the apparatus is expensive to maintain high pressure and high speed, and there are various limitations in securing an efficient processing amount due to having a narrow flow path and a nozzle portion. What is common to these two types of equipment is that they utilize high energy, increase the temperature during processing, and depending on the type of substance that constitutes the liquid material, there may be denaturation or reagglomeration, etc. In practice, there are many restrictions on substances to be applied, application conditions, and the like.

[0005]

SUMMARY OF THE INVENTION The present invention is to provide an emulsifying and dispersing apparatus for efficiently and stably dispersing or emulsifying while utilizing the usefulness of the above apparatus.

[0006]

According to the present invention, there is provided (1) a method of emulsifying or dispersing a liquid or a solid (a) in a mixture of a liquid or a solid (a) and a liquid (b) into fine particles. Wherein the mixture is passed through one or two or more pores having a diameter of 0.1 to 5 mm (inner diameter), (2) behind the pores, 2. The emulsifying and dispersing device according to claim 1, wherein the front portion has a resistive body having a conical shape or the like, which obstructs the flow of the mixture, (3) the inner wall of the pore portion has a spiral groove, concave or convex resistive shape. 3. The emulsifying and dispersing apparatus according to claim 1, wherein (4) the pore portion has a tapered shape in which a diameter gradually increases at a front portion thereof and gradually decreases at a rear portion thereof. The emulsifying and dispersing apparatus according to (5), wherein the pores are cooled near the pores. The emulsifying and dispersing device according to any one of claims 1 to 4, further comprising a cooling device that performs the operation, (6) the ultrasonic vibrating device provided near or behind the pore portion. Emulsifying and dispersing equipment,
(7) The emulsifying and dispersing apparatus according to any one of claims 1 to 6, wherein a pressure of 5 to 1000 kg / cm ² is applied to the mixture to pass through the pores.

[0007]

BEST MODE FOR CARRYING OUT THE INVENTION In the emulsifying and dispersing apparatus of the present invention,
When the liquid mixture passes through the pores at a relatively high speed, phenomena such as collision, impact, and shear occur in the liquid mixture, and fine emulsification and dispersion are performed. The pore diameter is 0.1
５5 mm. If the diameter of the pores is smaller than 0.1 mm, the resistance to the flow of the mixture becomes strong, and especially in the case of a liquid containing fine particles at a high concentration or a liquid having a high viscosity, is the flowability significantly inhibited? Even if the fluidity is maintained, even though the varnish component of the mixture passes, the fine particles do not pass, and there is a risk of causing accumulation and aggregation. If the diameter is larger than 5 mm, it is difficult to obtain a flow at a high pressure and a high flow rate, and the effect of collision and dispersion is reduced. For effective emulsification and dispersion, the thickness is more preferably 0.5 to 2 mm.

In the present invention, the flow path of the liquid material has a diameter of 2 to 20 mm in front of and behind the fine pore portion (if there is a resistor), more than twice the diameter of the fine pore portion. preferable. If it is smaller than 2 mm, the resistance to the flow of the liquid increases, and the flow of the liquid of high concentration and high viscosity, which is one of the objects of the present invention, requires a large energy loss and requires a large power. If the diameter is larger than 20 mm, the step with the pore diameter becomes too large, which may obstruct the flow. If the step is reduced, it becomes difficult to obtain the required pressure and flow rate, and the dispersing effect tends to be impaired. In addition, the diameter of the pore portion is 2
If it is less than twice, the effect of collision and dispersion in the pores tends to be insufficient. The pore portion preferably has a spiral or uneven resistance shape on the inner wall thereof. Due to such a resistance shape, a phenomenon of greater stirring and shearing occurs, and the effect of dispersion is further enhanced. The tapered shape whose diameter gradually changes before and after the pore portion, that is, from the rear portion of the inflow portion to the pore portion and from the pore portion to the outflow chamber, impedes the flow of the liquid material, and may cause a failure of the device. It is preferable to reduce unnecessary resistance that may be caused.

Behind the pores, impedes the flow of the mixture,
By providing a resistor having a conical front portion or the like, the liquid mixture collides with the tip of the resistor and in the vicinity thereof, and a shearing force is applied to further finely emulsify and disperse. In addition to the conical shape at the front portion, the shape of such a resistor may be a pyramid shape, a truncated cone shape having a flat entire surface, a truncated pyramid shape, or a shape in which a groove is provided along the flow direction. The shape is not particularly limited as long as the liquid mixture that has passed through the holes collides with the resistor and a fine emulsification and dispersion is performed by the impact or shear force at that time.

When the flow of the liquid mixture is hindered due to the high viscosity, or when there is a possibility that the components may be separated, a screw type or vibration type conveying means is connected to the inlet side of the emulsifying and dispersing apparatus of the present invention. Thereby, the above-mentioned problem is solved, and the flow and the stirring are performed without any problem. For the treatment of liquid mixtures containing substances that are expected to undergo thermal deterioration or reagglomeration, a cooling device connected to a cooling pipe connected to a cooler for cooling the vicinity of the pores shall be provided. Thereby, stable processing can be performed. Further, an ultrasonic vibration device is provided in the pore portion or behind the same, and by applying ultrasonic vibration to the mixture after emulsification and dispersion, the emulsification and dispersion effect can be further increased and reagglomeration can be reduced, so that the emulsification and dispersion state can be improved. It can be kept better.

When the liquid mixture is treated with the emulsifying and dispersing apparatus of the present invention, in order to perform effective emulsifying and dispersing, 5 to 1
It is preferable to apply a pressure of 000 kg / cm 2 to allow the pores to pass. At 5kg / cm2, collision, impact,
If the shearing force exceeds 1000 kg / cm2, the impact and the shearing are too strong, the temperature rises sharply, and there is a possibility that denaturation and deterioration may occur depending on the substance.
If the viscosity is relatively high or higher, the energy efficiency is poor. More preferably, it is 200 to 800 kg / cm2. However, relatively low viscosity or 30% fine particle content
In some cases, it is effective to emulsify, disperse, and the like by setting the pressure to a level lower than or equal to a higher pressure.

[0012]

DESCRIPTION OF THE PREFERRED EMBODIMENTS The present invention will be described below with reference to the illustrated embodiments. FIG. 1 is a flow chart of the emulsifying and dispersing apparatus (one example) of the present invention, which is preferably applied when the liquid mixture has a high viscosity. The liquid mixture (a) is transported to the pressurizing section (2) by the conveying means (1), and is pressure-fed to the pore section (4) via the inflow section (3) by a high-pressure pump (11) or the like. The liquid mixture (a), when passing through the pores (4),
Emulsification / dispersion is performed by shearing or the like. Then, it reaches the outflow section (6) via the outflow chamber (5). Pore part (4)
A cooling device (12) and a cooling pipe (13) connected to the cooling device (12) are provided in the vicinity thereof. The outflow chamber (5) is provided with an ultrasonic irradiation device (14) as required. Further, the outflow portion (6) may be configured to pass through the refrigerant, for example, as a spiral pipe.

FIG. 2 is a schematic sectional view of an emulsifying and dispersing apparatus (one example) of the present invention. The liquid mixture (a) is transferred to the pressurizing section (2) by the conveying means (1). The pressurizing section (2) has check valves (2a) and (2b) at its inlet and outlet. Next, the high pressure pump (11) feeds the pressure to the pores (4) through the inflow section (3) where the diameter of the rear part is reduced in a tapered shape. When the liquid mixture has a high viscosity of about 300 poise, the pressure is 300 to 1000 kg / cm ² and the inflow section (3)
Has a diameter of 2 to 10 mm, and the pore portion (4) has a diameter of 0.5 to 10 mm.
It is preferably about 1.5 mm. Two or more pores (4) may be provided. In this case, emulsification and dispersion by impact and shear in the pores and the outflow chamber (5) can be performed more effectively.

When the liquid mixture flowing out of the pores (4) at a relatively high speed flows into the outflow chamber (5), the liquid mixture collides with the resistor (7) having a conical front portion and the outer periphery of the resistor. Divides and expands along the part, flows and merges again. Uniform dispersion and emulsification are performed by these series of collision, shear, expansion, and merging. The resistor (7) having a conical front portion as shown in the figure is the most preferable example in consideration of impact, shearing or fluidity of liquid. Subsequently, an ultrasonic irradiation device (14) provided at the rear of the outflow chamber (5)
, The dispersion / emulsification is promoted and flows out to the outflow portion (6). Ultrasound irradiation is preferably performed by a method in which a horn is surrounded by a cartridge so that uniform processing can be performed, and irradiation is performed from the tip of the horn. A cooling device (12) and a heat transfer portion (13) such as a cooling pipe through which a refrigerant is connected are installed in and around the pore portion (4).

FIG. 3 is an enlarged sectional view of the pore portion and the outflow chamber in FIG. The liquid mixture (a) passes through the pore portion (4) via the inflow portion (3) and collides with the resistor (7), and the flow is reduced by a tapered outer peripheral path (15) on the outer periphery of the resistor (7). ) And (16), the material is once expanded and narrowed by merging again, so that collision, shear, and dispersion are effectively performed, and fine and uniform emulsification and dispersion are performed. A spiral rib (17) or the like is provided on the resistor (7) if necessary.
Shearing and dispersion can be performed more effectively.
By providing the resistor (7), the outer diameter of the flow path is larger than that of the fine pores (4), but the expanded outer diameter of the flow path is preferably at least twice the diameter of the fine pores.

FIG. 4 is an enlarged cross-sectional view of the pore portion, in which the pore portion (4) has a resistance shape formed by a spiral groove (18). In the figure, a spiral groove is formed on the inner wall over the entire length of the pore portion, and the liquid mixture is
When passing through the pore portion (4) having the helical groove via the inflow portion (3), it is dispersed and emulsified by stronger collision / shear and reaches the outflow chamber (6). Such a resistance shape may be a spiral groove, a rod-shaped, flat-plate-shaped convex part, or a rectangular or circular concave part.

When a specific example of such an emulsifying and dispersing apparatus is used, a varnish containing a liquid epoxy resin as a main component is used in an amount of 0.1 to 0.1%.
500 kg / cm ^{2 of} a paste having a viscosity of about 300 cp or more in which 30 μm fine particles are mixed at a ratio of 50 to 95%.
Observed with an electron microscope, the fine particles hardly aggregated, the dispersion state was very good, and reagglomeration was substantially maintained even after a long time (one month) after the treatment. I didn't see it.

[0018]

The emulsifying and dispersing apparatus of the present invention can stably disperse fine particles and finely emulsify and disperse even a high-viscosity liquid mixture containing fine particles. In addition, it is an emulsifying and dispersing apparatus that is excellent in stability and practicality because it can prevent deterioration and re-aggregation of the substances constituting the mixture.
The emulsifying and dispersing device of the present invention performs efficient emulsification and dispersion by providing micro resistance with respect to the flow of a liquid mixture and ensuring a good flow on a macro scale.

[Brief description of the drawings]

FIG. 1 is a flowchart of an emulsifying and dispersing apparatus (one example) of the present invention.

FIG. 2 is a schematic sectional view of an emulsifying and dispersing apparatus (one example) of the present invention.

FIG. 3 is an enlarged sectional view of a pore portion and an outflow chamber in FIG. 2;

FIG. 4 is an enlarged cross-sectional view of FIG. 2 when the pores have a resistance shape;

[Explanation of symbols]

 a Liquid mixture 1 Conveying means 2 Pressurizing section 2a Inlet check valve 2b Outlet check valve 3 Inflow section 4 Porous section 5 Outflow chamber 6 Outflow section 7 Resistor 11 High pressure pump 12 Cooling device 13 Heat transfer section 14 Ultrasonic irradiation Zones 15, 16 Tapered peripheral path 17 Spiral rib 18 Spiral groove

Claims (7)

[Claims] 1. A method of micronizing a liquid or a solid (a) in a mixture of a liquid or a solid (a) and a liquid (b) and emulsifying or dispersing the mixture in the liquid (b), wherein the mixture has an inner diameter of 0.1 to 5 mm. An emulsifying and dispersing apparatus characterized by passing through one or two or more pores having 2. The emulsifying and dispersing apparatus according to claim 1, further comprising a resistive element having a conical shape at a front portion thereof, which obstructs the flow of the mixture behind the fine pores. 3. The emulsifying and dispersing apparatus according to claim 1, wherein the inner wall of the fine pore portion has a spiral groove, a concave or a convex resistance shape. 4. The emulsifying and dispersing apparatus according to claim 1, wherein the fine pore portion has a tapered shape in which a diameter gradually increases at a front portion thereof and gradually decreases at a rear portion thereof. 5. The emulsifying and dispersing apparatus according to claim 1, further comprising a cooling device provided near the pores for cooling the pores. 6. The emulsifying and dispersing apparatus according to claim 1, wherein an ultrasonic vibrator is provided near or behind the pores. 7. The emulsifying and dispersing apparatus according to claim 1, wherein a pressure of 5 to 1000 kg / cm ² is applied to the mixture to pass through the pores.