JPH0889774A - Emulsifying and dispersing method and emulsifying and dispersing device - Google Patents

Abstract

PURPOSE: To continuously produce a good-quality emulsified and dispersed product having a small grain diameter and narrowed in a grain size distribution range, to easily adjust the mixing ratio and to perform quick treatment before a reaction occurs. CONSTITUTION: This emulsifying and dispersing method is to supply a main liq. to the treating space on which specified high pressure, shearing force and shearing stress are exerted, then directly supply an auxiliary liq. to the treating space and continuosuly treat to prepare an emulsified and dispersed liq. In the emulsifying and dispersing device 21, a multistage annular stator 31 having slits and a multistage rotor 49 combined with the stator 31 are coaxially provided, and feed passages 27 and 45 are connected for each liq. to be mixed to the treating space formed by a combination of the stator 31 and rotor 49.

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 method and an emulsifying and dispersing apparatus for emulsifying two or more kinds of liquids or for dispersing one or more kinds of liquids and a solid suspension mixed with another liquid. Regarding

[0002]

2. Description of the Related Art Conventionally, an emulsifying and dispersing method for two or more kinds of liquids and an emulsifying and dispersing apparatus have been used in various fields. Recently, there are fields in which heavy oils such as oil sand oil and petroleum asphalt are used as fields in which the emulsion dispersion method is used. Originally, these heavy oils are widely distributed in each region of the world and are known to have reserves equal to or higher than petroleum. Further, petroleum itself tends to be converted into heavy oil in the future, and asphalt generated from the crude oil refining process is also increasing, so demand expansion is demanded.

However, these heavy oils have a softening point above room temperature and become solid or semi-solid at room temperature, and are difficult to handle, so that their applications are limited. On the other hand, when these heavy oils are emulsified into oil-in-water type emulsions, the viscosity is lowered and the handling at room temperature becomes easy. In the case of producing an emulsion consisting of one phase by emulsifying two or more kinds of liquids having low mutual solubility,
Alternatively, when a dispersion product is produced from one or more kinds of liquid and a fixed suspension mixed with another liquid, conventionally, a tank-type stirrer, an emulsifier such as a Harrel-type homogenizer or a colloid mill is used. Was there.

FIG. 7 is an explanatory diagram of a method for producing an emulsified product when a tank-type stirrer is used. In this conventional example, two or more kinds of low-solubility liquids A and B, which are raw materials, are put into the stirring tank 1, and after stirring for a long time by the rotor blades 3, the product C is extracted from the stirring tank 1. .

FIG. 8 is an explanatory diagram of a method for producing an emulsified product when an emulsifying machine is used. In this conventional example, a T-type branch pipe (or Y-type branch pipe) 7 is connected to a raw material supply port of a high-speed rotary emulsification disperser 5 having a stator and a rotor, and a T-type branch pipe 7
Is connected to tanks 9a and 9b in which a main liquid D and a sub liquid E having a predetermined ratio are separately charged. The pumps 11a and 11 provided in the supply pipes from the tanks 9a and 9b, respectively.
In b, a predetermined amount of raw material is simultaneously supplied to the high-speed rotary emulsifying disperser 5, and the discharged product F is again supplied to one of the tanks 9a and 9b.
The raw material was circulated by being returned to.

[0006]

However, in the method for producing an emulsified product using the tank-type stirrer described above, stirring is generally performed at room temperature, and since it is an open system and no pressure is applied, fine particles are not used. Was difficult to obtain and the particle size range was wide. Further, since the material is so-called batch type in which the material is stirred once, there is a problem that the material cannot be continuously processed.

On the other hand, in the method for producing an emulsified product using the above-mentioned high-speed rotary emulsification disperser 5, although heating and pressurization are easy, if the raw material ratio deviates greatly from 1: 1, the branch pipe (T Type or Y-shaped branch pipe) 7 makes it difficult to mix the raw materials rapidly and uniformly, and the particle size does not become as fine as expected. In addition, this manufacturing method also uses the discharge product F.
Since the circulation process is performed again for returning to the tank 9a, 9b, the process is basically a batch process, and there is a problem that the raw material cannot be continuously processed as in the above method. Furthermore, in this case, before the supply to the high-speed rotary emulsification disperser 5, the branch pipe 7
Since the raw materials D and F join together, the contact time after the joining until the raw material flows into the high-speed rotary emulsification disperser 5 is too long depending on the physical properties of the raw materials, and the reaction causes a large particle size. There was also a problem that products with the required particle size could not be obtained.

The present invention has been made in view of the above circumstances, and it is possible to continuously produce a high-quality emulsified dispersion product having a small particle size and a narrow particle size range, and it is easy to adjust the mixing ratio, and the reaction It is an object of the present invention to provide an emulsifying and dispersing method and an emulsifying and dispersing apparatus that enable quick processing before the occurrence.

[0009]

An emulsifying and dispersing method according to the present invention for achieving the above object is to supply a main liquid to a specific processing space to which a predetermined high pressure, shearing force and shear stress are applied, The method is characterized in that an emulsified dispersion liquid is produced by continuous processing while directly supplying a sub liquid to this processing space. Further, the emulsification dispersion device is provided with a multi-stage ring-shaped stator having a slit and a multi-stage ring-shaped rotor having a structure having a slit, which is complementarily combined with the slit of the multi-stage ring-shaped stator, on the same axis. A separate supply path for each mixed liquid is connected to a processing space formed by a combination of a stator and a rotor.

[0010]

In the emulsification dispersion method, in a specific processing space,
The secondary liquid is directly supplied to the main liquid to which a predetermined high pressure, shearing force and shear stress have been applied, and at the same time as the mixing, the both mixed liquids are continuously processed by the shearing force and shear stress to be emulsified and dispersed. As a result, even in a raw material in which a reaction occurs even if the contact time is short, the contact time before mixing is eliminated and the reaction does not occur. In the emulsification dispersion device, in the processing space formed by the multistage ring-shaped stator and the multistage ring-shaped rotor,
Separate supply paths are connected to the mixed liquids, and the mixed liquids are mixed for the first time in the processing space, so that there is no contact between the mixed liquids before the processing.

[0011]

The preferred embodiments of the emulsifying and dispersing method and the emulsifying and dispersing apparatus according to the present invention will be described below with reference to the drawings. FIG.
2 is a sectional view of a main part of the emulsifying and dispersing apparatus according to the present invention, FIG. 2 is a sectional view of a stator, FIG. 3 is a plan view of a processing surface side of the stator, FIG. 4 is a plan view of a back surface side of the stator, and FIG. It is a principal part enlarged view of an emulsification dispersing device. A casing 23 is provided in the emulsification / dispersion device 21, and the casing 23 has a cylindrical housing chamber 25 therein. A raw material inlet (supply port) 27 is provided at the center of one circular inner wall of the storage chamber 25, and the raw material inlet 27 penetrates into the storage chamber 25 from the outside. A product outlet 29 is provided on the peripheral side wall of the storage chamber 25 sandwiched between the two circular inner walls, and the product outlet 29 penetrates from the storage chamber 25 to the outside.

A multi-stage ring-shaped stator (hereinafter referred to as "stator") 31 is fixed to one circular inner wall of the storage chamber 25 at the same center, and the center of the stator 31 communicates with the raw material inlet 27. It is 33 and opens. As shown in FIG. 2, on the circular surface (processing surface) of the stator 31 opposite to the one circular inner wall, annular projections SI and S concentric with the stator 31 are formed.
II and SIII are projected in a multi-stepped manner (three steps in this embodiment), and the gaps between the annular projections SI, SII and SIII form circumferential grooves 35 and 37. Each annular protrusion S
A plurality of slits 39 traversing in the radial direction are formed in I, SII, and SIII, and the space formed by the slits 39 is a so-called chamber.

A peripheral groove 3 which is a gap between the annular projections SI and SII.
A plurality of secondary liquid ejection holes 41 (6 in this embodiment)
4) are formed by equally dividing the circumference, and the auxiliary liquid ejection holes 41 are formed in FIG.
Is communicated with an annular sub liquid distribution groove 43 formed on the surface (rear surface) opposite to the processing surface of the stator 31 shown in FIG. The sub liquid distribution groove 43 is closed when the stator 31 is fixed to the circular inner wall of the accommodation chamber 25, and communicates with the outside in accordance with the sub liquid inlet (supply passage) 45 provided in the casing 23. Further, any number of the sub liquid ejection holes 41 can be closed. As means for closing the sub liquid jetting hole 41, although not shown, a needle valve structure in which a needle pin is inserted from the sub liquid distribution groove 43 side, or a shutter in which holes of substantially the same diameter are formed is used. It is conceivable that the opening degree of the sub liquid ejection hole 41 can be varied by sliding it relative to the sub liquid ejection hole 41.

On the other hand, a drive shaft 47 is rotatably supported at the center of the other circular inner wall of the storage chamber 25, and the drive shaft 47 is connected to a drive unit (not shown) and is rotated at a high speed. A multi-stage ring-shaped rotor (hereinafter referred to as “rotor”) 49 is fixed to the tip of the drive shaft 47, and the rotor 49 is arranged parallel to the stator 31 and on the same central axis. As shown in FIG. 5, the stator 31
Ring projections RI, RII, RIII, and RIV, which are concentric with the rotor 49, are provided on the facing surface of the rotor 49, which is opposed to, in a multi-stepped manner (four steps in this embodiment).
II, RIII and RIV are surrounded by circumferential grooves 51, 53,
Forming 55. In addition, each annular protrusion RI,
For RII, RIII, and RIV, like the stator 31,
A plurality of slits 57 are formed so as to traverse in the radial direction.

The stator 31 and the rotor 49 have annular projections SI, SII, SIII and circumferential grooves 35, 37, and annular projections RI, RII, RIII, RIV and circumferential grooves 51, 5 respectively.
3, 55 are combined with each other (complementary). Therefore, the combination of the stator 31 and the rotor 49 forms a processing space 59, which is a small gap, between the annular projections SI, SII, SIII and the annular projections RI, RII, RIII, RIV. ing.

FIG. 6 is a diagram for explaining the flow of raw materials in the present invention. Emulsifying and dispersing device 21 configured as described above
The main liquid G from the main liquid tank 61 is supplied to the raw material inlet 27 by the main liquid pump 63. In addition, the auxiliary liquid H from the auxiliary liquid tank 65 is introduced into the auxiliary liquid inlet 45 of the emulsifying and dispersing apparatus 21.
Are supplied by the sub liquid pump 67. Then, the main liquid G and the sub liquid H supplied to the emulsification / dispersion device 21 are emulsified and dispersed by the action described later to become the product J and the product outlet 2
Taken out from 9.

Next, the operation of the emulsification / dispersion device 21 configured as described above will be described. As shown in FIG.
Is rotated at a high speed, and the main liquid inlet 33 of the stator 31 is rotated.
When the main liquid is supplied into the slits 57 of the rotor 49 from the main liquid inlet 33, the main liquid G is discharged from the outer circumference of the annular projection RI by the centrifugal force, and the first inner stage of the stator 31 is discharged. After being pressed against the annular projection SI, the slit 39 of the annular projection SI enters. The main liquid G entering the slit 39 is
It is pushed by the main liquid G sequentially discharged from the outer circumference of the annular projection RI by centrifugal force, and is further discharged into the processing space 59 which is a gap between the circumferential groove 35 and the annular projection RII.

At the same time, the sub-liquid H is supplied from the sub-liquid jetting hole 41 opened on the bottom surface of the peripheral groove 35 through the sub-liquid distribution groove 43, and the main liquid G in the processing space 59 and the sub-liquid H are supplied. Combine to form a mixed solution. At this time, a strong shearing force is applied to the mixed liquid by the annular projections SI and SII of the stator 31 and the annular projection RII of the rotor 49, and the axial direction and the radial direction of the stator 31 and the rotor 49 are applied. The shear stress is applied as it passes through the gap. That is, a strong shearing force and shear stress are applied to the mixed liquid at the same time as the merging.

The adjustment of the inflow rate of the sub liquid H can be easily achieved by closing some of the sub liquid jet holes 41 having a plurality of openings or by reducing the area. This is compared with the conventional method in which the auxiliary liquid to be supplied to the branch pipe is adjusted by controlling the discharge pressure or the flow rate of the pump, but the opening / closing number control or the opening degree of the auxiliary liquid ejection holes 41 is maintained under a constant pressure. This is because more stable flow velocity can be obtained by controlling.

After the shearing force and shear stress are applied, the mixed liquid is pushed by the later mixed liquid and enters the slit 39 of the annular projection SII to be opened. As a result, the mixed solution becomes
It will also be subject to pressure changes at high frequency levels. The mixed liquid that has entered the slit 39 of the annular projection SII undergoes similar shearing force, shear stress, and high-frequency level pressure change, and the outer annular projections SII and SIII and the annular projections RII and RII.
While receiving repeatedly in the processing space 59 with I and RIV,
It is moved to the outside and finally the emulsification and dispersion are completed.
And is taken out from the product outlet 29.

According to the emulsification / dispersion method using the above-mentioned emulsification / dispersion device 21, the sub-liquid jet holes 41 are directly opened in the processing space 59, and at the same time as the main liquid G and the sub-liquid H are joined, a strong shearing force and Since the shear stress is applied, a high-quality emulsified dispersion product having a small particle size and a narrow particle size range can be continuously produced. In addition, a quick reaction without reaction can be performed, and a product having a small particle size and a narrow particle range can be obtained even in a difficult material in which a reaction occurs when the contact time of the raw material is long. Further, by closing some of the auxiliary liquid ejection holes 41 or reducing the area, the inflow speed of the auxiliary liquid can be adjusted easily and accurately, so that the ratio of the main liquid and the auxiliary liquid is greatly deviated from 1: 1. Even the secondary liquid can be quickly and uniformly mixed, and can be instantly emulsified and dispersed to obtain a high-quality product.

Next, using the emulsifying and dispersing device 21 described above,
The results of an experiment conducted for the purpose of obtaining a fine particle resin dispersion product having an average particle size of about 5 μm are shown below.

The resin liquid was obtained by dissolving resin in oil, and the ratio of resin to oil was half. The emulsified liquid was prepared by dissolving a surfactant in ion-exchanged pure water so as to have a pure concentration of 1%.

The liquid flow rates of the emulsified liquid and the resin liquid are 360 liters and 24 liters per hour,
The amount of product was adjusted to 384 liters per hour. Therefore, the volume mixing ratio in this case is 1 for the resin liquid with respect to the emulsion 15. Further, the surfactant is added in an amount of 15% of pure content in the sub liquid and 30% of pure content in the resin.

In this treatment, the resin is first atomized by the action of the surfactant in the emulsion and the shearing force applied from the emulsifying / dispersing device 21, but the resin itself does not dissolve in water, so in water. Present as fixed microparticles, the product is obtained as a dispersion.

As the emulsifying / dispersing device 21, a Cavitron (trade name) CD1010 type manufactured by Nittetsu Mining Co., Ltd. was used. The specific specifications are shown below. The rotor has four stages with an outer diameter of 35 to 74 mm, a slit number of 12 to 72, and a slit width of 3.0 to 0.6 mm. The stator has three stages with an outer diameter of 46 to 68 mm, a slit number of 24 to 72, and a slit width of 2.0 to 0.6 mm.

(Experiment 1) A volume of 15 liters of the emulsion is 20
The mixture was charged into a liter emulsion tank, and supplied from the emulsion pump to the raw material inlet of the Cavitron CD1010 type (hereinafter referred to as "emulsion dispersion device"). On the other hand, 2 liters of the resin liquid was charged into a resin liquid tank having a volume of 5 liters and was supplied to the sub liquid inlet by a resin liquid pump. The rotor of the emulsifying and dispersing device is 11200
After operating at rpm, the emulsion was sent at a rate of 6 liters per minute from the emulsion pump, and 0.4 minutes per minute from the resin liquid pump.
The resin solution was sent in liters and the product was received in another 20 liter product container. Therefore, in this case, the raw material passes through the emulsifying and dispersing apparatus only once. In this experiment 1, the secondary liquid ejection holes were opened from the inside of the stator between the first and second annular projections and between the second and third annular projections. It also compared with the case. In this case, the auxiliary liquid ejection hole had a diameter of 2 mm. The comparison is
The product was taken out and the particle size was measured by a laser diffraction particle size analyzer (Microtrac FRA type). The results are written as representative particle diameters corresponding to 10%, 50%, 90%, and 100% of the passing amount (d ₁₀ , d ₅₀ , d ₉₀ , and d ₁₀₀ , respectively,
The units are arranged in μm) and shown in Table 1.

[0028]

[Table 1]

(Experiment 2) Of the stators of the emulsifying and dispersing apparatus,
2mm in diameter from the inside to the space between the 1st and 2nd step ring protrusions
By opening six sub liquid ejection holes at equal intervals and closing some of the sub liquid ejection holes or reducing the area, the sub liquid ejection holes can be discharged from the sub liquid ejection holes for the same sub liquid inflow amount. The inflow velocity U of V was changed. In this case, 1 in the stator
The cross-sectional area of the main protrusion passage of the annular projection of the step is 120 mm ² , and the main liquid passage velocity V is 0.83 m / s. In the calculation example, V = 360 l / h / 1000 / (3600s / hx120mm ² /1000000)=0.83m/s
Is. Further, with respect to the auxiliary liquid inflow amount of 24 liters / hour, the auxiliary liquid inflow velocity U when some of the auxiliary liquid ejection holes are closed is that the passage cross-sectional area of the auxiliary liquid ejection hole is 3.14 mm ^2. , 2.1 m / s. If it is shown by a calculation example, U = 24 l / h / 1000 / (3600s / hx3.14mm ² /1000000)=2.1m/s
Is. From the above, Table 2 shows the relationship between the cross-sectional area of passage of the secondary liquid ejection holes and the secondary liquid inflow speed, and Table 3 shows the relationship between the secondary liquid inflow speed and the particle size.

[0030]

[Table 2]

[0031]

[Table 3]

From the above experimental results, even when the raw material ratio greatly deviates from 1: 1, the structure based on the emulsification / dispersion device 21 of the above-described embodiment is used, the main liquid inlet and the sub liquid jet hole can be used to discharge the main liquid. The particle size of the product was measured as d
_{As shown at 90} = 4.9 μm (first to second stages), it was confirmed that the expected product was obtained. Further, in this case, it has been found that it is desirable to open the secondary liquid ejection holes between the first stage and the second stage of the stator. Further, good results are obtained by setting the auxiliary liquid inflow velocity U within a certain range with respect to the main liquid passage velocity V, and the velocity ratio U / V thereof.
As shown in Table 3, a value between 0.9 and 1.9 is desirable, and as a means for setting the sub liquid inflow velocity within this range, some of the plurality of sub liquid ejection holes are closed or the area is adjusted. It was confirmed that it can be used.

The emulsifying and dispersing device 2 according to the above-mentioned embodiment
In 1, the plurality of sub liquid ejection holes 41 are connected to one sub liquid distribution groove 43.
The case in which one type of sub liquid is supplied from the sub liquid ejection hole 41 through the sub liquid distribution groove 43 has been described as an example, but the emulsification dispersion device 21 divides the sub liquid distribution groove 43 and divides it. Separate sub liquids may be supplied from the respective sub liquid distribution grooves 43. Further, in this case, the sub liquid distribution groove 43
May be divided in the circumferential direction, or may be divided into concentric multi-step grooves.

[0034]

As described in detail above, according to the emulsification / dispersion method of the present invention, the main liquid is supplied to a specific processing space to which a predetermined high pressure, shearing force and shear stress are applied. Since it was decided to carry out continuous processing while directly supplying the by-liquid to the processing space, the contact time before mixing was eliminated, and the reaction did not occur even in the raw material where the reaction occurred even with a short contact time, and the particle size was small and the particle size range was small. It is possible to continuously produce a high quality emulsified dispersion product which is narrow. According to the emulsification disperser, the multistage ring-shaped stator having the slit and the multistage ring-shaped rotor also having the slit are coaxially provided, and mixed in the processing space formed by the combination of the stator and the rotor. Since the separate supply paths are connected for each liquid, the contact between the mixed liquids before the treatment is eliminated, and the raw material can be quickly treated before the reaction occurs.

[Brief description of drawings]

FIG. 1 is a sectional view of an essential part of an emulsifying and dispersing apparatus according to the present invention.

FIG. 2 is a sectional view of a stator.

FIG. 3 is a plan view of a processing surface side of a stator.

FIG. 4 is a plan view of the back surface side of the stator.

FIG. 5 is an enlarged view of a main part of an emulsification dispersion device.

FIG. 6 is a diagram illustrating a flow of raw materials in the present invention.

FIG. 7 is an explanatory diagram of a method for producing an emulsified product when a tank stirrer is used.

FIG. 8 is an explanatory diagram of an emulsified product manufacturing method using an emulsifying machine.

[Explanation of symbols]

 21 Emulsifying and Dispersing Device 27 Raw Material Inlet (Supply Pass) 31 Multi-Stage Ring-Shaped Stator 33 Main Liquid Inlet 39, 57 Slit 41 Spouting Hole 43 Distribution Groove 45 Sub-Liquid Inlet (Supply Pass) 49 Multi-Stage Ring-Rotor 59 Processing Space

Claims (5)

[Claims] 1. A main liquid is supplied to a specific processing space to which predetermined high pressure, shearing force and shear stress are applied, and
An emulsification dispersion method characterized in that continuous processing is performed while directly supplying a sub-liquid to the processing space to prepare an emulsion dispersion. 2. A multi-stage ring-shaped stator having a slit, and a multi-stage ring-shaped rotor having a structure having a slit, which is complementary to the slit of the multi-stage ring-shaped stator, are provided coaxially. An emulsification / dispersion device characterized in that separate supply paths are connected to each of the mixed liquids in a processing space formed by a combination of a stator and the rotor. 3. A distribution groove connected to at least one liquid supply path is formed in the stator along the processing space,
The emulsifying and dispersing apparatus according to claim 2, wherein an auxiliary liquid ejection hole that connects the distribution groove and the processing space is formed in the stator. 4. The main liquid inlet is provided in the vicinity of the center of the stator, and the auxiliary liquid ejection hole is arranged radially outward of the stator with respect to the main liquid inlet. Emulsifying and dispersing device. 5. The emulsifying / dispersing device according to claim 3, wherein any of a plurality of the sub liquid ejection holes is provided so as to be closed.